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DR ANTHONY MELVIN CRASTO,WorldDrugTracker, helping millions, A 90 % paralysed man in action for you, I am suffering from transverse mylitis and bound to a wheel chair, With death on the horizon, nothing will not stop me except God................DR ANTHONY MELVIN CRASTO Ph.D ( ICT, Mumbai) , INDIA 25Yrs Exp. in the feld of Organic Chemistry,Working for GLENMARK GENERICS at Navi Mumbai, INDIA. Serving chemists around the world. Helping them with websites on Chemistry.Million hits on google, world acclamation from industry, academia, drug authorities for websites, blogs and educational contribution

Thursday, 8 January 2015

3,3-Dicarbethoxy-3,4-dihydro-9-(1-methylethylidene)-1,4-methano-1H-2-benzopyran

3,3-Dicarbethoxy-3,4-dihydro-9-(1-methylethylidene)-1,4-methano-1H-2-benzopyran
37

3,6-Di(2-pyridyl)stetrazine (0.45g; 1.9 mmol) was added slowly to a stirred solution of the hydrocarbon 33 (0.30g; 1.6 mmol) and diethyl oxomalonate 36(0.25 ml); 1.6 mmol) in chloroform (10 ml) and the resulting solution stirred for 1 hour. Removal of the solvent afforded the crude product. Attempts to purify this product by chromatography on silica gel or alumina only resulted in its rearrangement. However, the p.m.r. spectrum (CDCl₃) of the product could be deduced from that of the crude compound: d 1.02 (3H, t J = 7 Hz, endo-OCH2CH3), 1.30 (3H, t J = 7 Hz), exo-OCH2CH3), 1.72 (3H, s, methyl protons), 1.76 (3H, s, methyl protons), 3.96 (2H, q J = 7 Hz, endo-OCH2CH3), 4.36 (2H, q J = 7 Hz, exo-OCH2CH3), 4.74 (1H, d Ja,b = 1.5 Hz, Hb) 5.76 (1H, d Ja,b = 1.5 Hz, Ha), 7.10-7.60 (4H, m, aromatic protons), and the mass spectrum showed the parent ion at m/e 330.

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1,1-Dimethyl-3,8-dihydro-1H-indeno[1,2-c]thiophen-3-one

1,1-Dimethyl-3,8-dihydro-1H-indeno[1,2-c]thiophen-3-one
3,6-Di(2-pyridyl)stetrazine (0.45g; 1.9 mmol) was added slowly to a stirred solution of the hydrocarbon 33 (0.30g; 1.6 mmol) and thiophosgene (0.125 ml; 1.6 mmol) in a 1:1 mixture of ethanol and chloroform (10 ml) and the resulting mixture stirred for 15 minutes. The solvent was removed and the residue partitioned between ether and water. The ethereal phase was washed with hydrochloric acid (3 x 20 ml; 0.5M) and water (2 x 10 ml), dried, and the solvent removed to yield the crude product. Purification by rapid preparative thinlayer chromatography (silica, chloroform/light petroleum 2:1) yielded a pale brown coloured oil which crystallized from ethanol. Recrystallization from ethanol afforded the product as clear, pale brown crystals (0.18g; 52%), m.p. 66-67 ^oC.
uv, visible spectrum: lmax 238, 243 (inf), 263 (inf), 300 (inf), nm; e 12650, 12080, 5120, 1490.
infra red spectrum: umax 1695 (s), 1315 (w), 1305 (m), 1270 (m), 1240 (m), 1200 (w), 1185 (w), 1145 (m), 1120 (m), 1080 (w), 1065 (m), 1015 (w), 870 (w), 855 (w), 835 (s), 780 (m), 760 (m), 720 (s), 690 (m) cm^-1.
P.m.r. spectrum (CDCl₃): d 1.82 (6H, s, methyl protons), 3.54 (2H, s, benzylic protons), 7.20-7.60 (3H, m, Hb), 7.70-7.90 (1H, m, Ha),
13C-[¹H] nmr spectrum (CDCl₃): d 29.12 (C9 & C10), 33.70 (C8), 55.90 (C1), 121.04 (C5), 124.91 (C6), 126.25 (C4), 127.12 (C7), 136.05 (C3b), 143.16 (C3a), 145.89 (C7a), 181.25 (C8a), 191.33 (C3).
Mass spectrum: m/e 217 (10%), 216 (M⁺, 61), 215(5), 201(15), 189(6), 188(29), 187(20), 183(9), 173(14), 171(6), 158(8), 157(26), 156(14), 155(33), 153(8), 152(7), 142(22), 141(18), 139(14), 130(6), 129(38), 128(19) 127(10), 116(7), 115(38), 114(20), 113(8), 102(7), 89(9), 88(7), 87(9), 86(8), 85(5), 79(9), 77(12), 76(10), 75(10), 74(10), 70(5), 69(5), 65(8), 64(10), 653(27), 62(13), 61(8), 59(100), 51(21), 50(11), 45(14), 41(12), 39(30), all other peaks less than 5%.
Analysis: Found: C, 71.9; H, 5.8, S, 14.9. C13H12OS requires C, 72.2; H, 5.6; S, 14.8%.

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2-Trimethylammonio-6-hydroxy-benzaldehyde oxime chloride

Peak assignment in the ¹H-NMR spectrum of 10 mM TAB2OH in 20 mM phosphate-pyrophosphate (+ 0.1 M NaCl) ²H₂O buffer, pH 5

2-Trimethylammonio-6-hydroxy-benzaldehyde oxime chloride (TAB2OH)

To a stirring solution of 4.19 (90 mg, 0.50 mmol) in dichloromethane (0.2 ml) at 0°C was added methyl trifluoromethansulfonate (62 μl, 0.55 mmol). The reaction was allowed to warm to room temperature and stirred for 40 h. The precipitate formed was collected by filtration washing with excess dichloromethane to afford 101 mg of the pure triflate salt as a white solid (59%). The salt was dissolved in acetonitrile and a solution of tetrahexylammonium chloride in acetonitrile was added to precipitate the pure chloride salt as a white solid.
¹H-NMR (600 MHz, d₆-DMSO) δ 11.74 (s, 1 H), 10.95 (s, 1 H), 8.34 (s, 1 H), 7.45 (t, J 8.4 Hz, 1 H), 7.39 (d, J 8.4 Hz, 1 H), 7.26 (d, J 8.2 Hz, 1 H), 3.68 (s, 9 H).

¹³C-NMR (150.9 MHz, d₆-DMSO) δ 158.9, 145.6, 145.5, 130.6, 117.5, 113.5, 111.3, 57.2.

HRMS (M⁺) expected, 195.1133; found, 195.1130.

http://www.biochemj.org/bj/450/bj4500231add.htm

MORE..............
2-Dimethylamino-6-hydroxy-benzaldehyde oxime (4.19)

To a stirring solution of 2-dimethylamino-6-methoxymethoxy-benzaldehyde oxime (14 mg, 0.06 mmol) in methanol (0.2 ml) at room temperature was added a 4 M solution of hydrogen chloride in dioxane (0.2 ml, 0.8 mmol). The reaction was heated to 70°C for 1 h and then cooled to room temperature and the solvent was blown off with nitrogen. The crude material was purified by flash chromatography over silica gel eluting with dichloromethane to afford 10 mg of pure product as a white solid (91%). ¹H-NMR (600 MHz, [²H]chloroform) δ 10.06 (s, 1 H), 8.65 (s, 1 H), 7.21 (t, J 8.1 Hz, 1 H), 7.11 (s, 1 H), 6.66 (d, J 8.2 Hz, 1 H), 6.60 (d, J 8.0 Hz, 1 H), 2.73 (s, 6 H). ¹³C-NMR (150.9 MHz, [²H]chloroform) δ 158.5, 154.8, 151.4, 131.6, 111.3, 110.2, 109.8, 45.6. HRMS (MH⁺) expected, 181.0971; found, 181.0983.

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1-pentyne

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A graph theory approach to structure solution of network materials from two-dimensional solid-state NMR data

A graph theory approach to structure solution of network materials from two-dimensional solid-state NMR data

Darren H. Brouwer and Kevin P. Langendoen

CrystEngComm, 2013,15, 8748-8762
DOI: 10.1039/C3CE41058G http://pubs.rsc.org/en/journals/articlecollectionlanding?sercode=ce&themeid=acb8167b-70f0-41f9-8ee8-e03bcf1367b9

An NMR crystallography strategy is presented for determining crystal structures of network materials such as zeolites from a single 2D NMR spectrum using concepts from graph theory.

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N,N-bis(5-methyl-2 hydroxybenzyl)methylamine (MMD)

1H NMR

Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

NOESY..........http://www.mdpi.com/1422-0067/12/7/4365/htm

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Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

Me

DR ANTHONY MELVIN CRASTO Ph.D ( ICT, Mumbai), INDIA, worlddrugtracker, 29Yrs Exp. in the field of Organic Chemistry,Working for GLENMARK PHARMA at Navi Mumbai, INDIA. Serving chemists around the world. Helping them with websites on Chemistry.Million hits on google, world acclamation from industry, academia, drug authorities for websites, blogs and educational content...........P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent. सुकून उतना ही देना प्रभू, जितने से जिंदगी चल जाये। औकात बस इतनी देना,कि औरों का भला हो जाये।

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Thursday, 8 January 2015

3,3-Dicarbethoxy-3,4-dihydro-9-(1-methylethylidene)-1,4-methano-1H-2-benzopyran

amcrasto@gmail.com

1,1-Dimethyl-3,8-dihydro-1H-indeno[1,2-c]thiophen-3-one

amcrasto@gmail.com

2-Trimethylammonio-6-hydroxy-benzaldehyde oxime chloride

amcrasto@gmail.com

1-pentyne

amcrasto@gmail.com

A graph theory approach to structure solution of network materials from two-dimensional solid-state NMR data

A graph theory approach to structure solution of network materials from two-dimensional solid-state NMR data

amcrasto@gmail.com

N,N-bis(5-methyl-2 hydroxybenzyl)methylamine (MMD)

amcrasto@gmail.com

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