3,5-Dimethylbenzenethiol → HCID 19365875, 화합물

HRID 849989노트

반응식

HRID 849989 반응식
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

참가 물질

6

반응물 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

생성물 1

HCID 19365875HCID 19365875, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-14b2803ebb0548299d13cc08434af730
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06015820

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