3,5-Dimethylbenzenethiol → Ethyl 4-[(3,5-dimethylphenyl)-thio]-1,6-dihydro-2-methyl-6-oxo-3-pyridinecarboxylate

HRID 1241535

반응식

HRID 1241535 반응식
Cl[C:2]1[C:3]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:4]([CH3:9])[NH:5][C:6](=[O:8])[CH:7]=1.[CH3:15][C:16]1[CH:17]=[C:18]([SH:23])[CH:19]=[C:20]([CH3:22])[CH:21]=1>C(O)C.C(N(CC)CC)C>[CH3:15][C:16]1[CH:17]=[C:18]([S:23][C:2]2[C:3]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:4]([CH3:9])[NH:5][C:6](=[O:8])[CH:7]=2)[CH:19]=[C:20]([CH3:22])[CH:21]=1

참가 물질

5

반응물 2

HCID 1175483,5-DimethylbenzenethiolHCID 21935322Ethyl 4-chloro-2-methyl-6-oxo-1,6-dihydro-3-pyridinecarboxylate

생성물 1

HCID 21935307Ethyl 4-[(3,5-dimethylphenyl)-thio]-1,6-dihydro-2-methyl-6-oxo-3-pyridinecarboxylate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

실험 절차

A mixture of the intermediate 13 (1.2 g; 5.6 mmol) in ethanol (15 ml), triethylamine (1.5 ml) and 3,5-dimethylthiophenol (1.45 ml; 11 mmol) was heated under reflux for 16 hours. After evaporation under reduced pressure, diethylether (50 ml) was added and the precipitate was filtered off. The intermediate 14 was obtained (1.42 g; 80%) as a colorless solid m.p.=233–235° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. customAfter evaporation under reduced pressure, diethylether (50 ml)
  4. additionwas added
  5. filtrationthe precipitate was filtered off

출처 및 근거

ORD 기록
ord-91805880c0424cffb923e923189a3dfb
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115608B2

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