3,5-Dimethylbenzenethiol → HCID 19365875、化合物

HRID 849989ノート

反応式

HRID 849989 の反応式
C[C:2]1[C:3]([S:12][C:13]2[CH:18]=[C:17](C)[CH:16]=[C:15](C)[CH:14]=2)=[C:4]([N+]([O-])=O)[C:5](=[O:8])[NH:6][CH:7]=1.C(C1C(SC2C=C(C)C=C(C)C=2)=C(C(OCC)=O)C(=O)NC=1C)C.CC1C=C(S)C=C(C)C=1>C(O)C.C(N(CC)CC)C>[C:13]1([S:12][C:3]2[CH:2]=[CH:7][NH:6][C:5](=[O:8])[CH:4]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

6

反応物 3

HCID 1175483,5-DimethylbenzenethiolHCID 4645742(1H)-Pyridinone, 4-((3,5-dimethylphenyl)thio)-5-methyl-3-nitro-HCID 4646013-Pyridinecarboxylic acid, 4-((3,5-dimethylphenyl)thio)-5-ethyl-1,2-dihydro-6-methyl-2-oxo-, ethyl ester

生成物 1

HCID 19365875HCID 19365875、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8471Triethylamine溶媒

実験手順

As for the method described for obtaining compound 7a in example 10, a mixture of compound 15 (1.00 g, 4.1 mmoles) in 10 ml of ethanol and 1 ml of triethylamine was agitated until homogeneous. 3,5-dimethylthiophenol (0.61 ml, 4.5 mmoles) was added. After 12 hours under reflux, the white precipitate was isolated by filtration and crystallised in ethyl acetate. Product 15 was obtained (1.05 g, 82%) in the form of white crystals: melting point 202° C.; NMR-1H (DMSO-d6) δ 12.17 (1H, s, NH-1), 7.22 (1H, s, H-4'), 6.92 (1H, s, H-2' and 6'), 4.09 (2H, q, J=7 Hz, COOCH2CH3), 2.45 (2H, q, J=7 Hz, CH2CH3), 2.27 (3H, s, CH3 -6), 2.25 (6H, s, CH3 -3' and 5'), 1.15 (3H, t, j=7 Hz, COOCH2CH3), 0.85 (3H, t, J=7 Hz, CH2CH3). Anal. C19H23NO3S (C, H, N, S).

後処理

  1. temperatureAfter 12 hours under reflux
  2. customthe white precipitate was isolated by filtration
  3. customcrystallised in ethyl acetate

出典と根拠

ORDレコード
ord-14b2803ebb0548299d13cc08434af730
出典データセット
uspto-grants-2000_01
特許番号
US06015820

反応ノート

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