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

HRID 1241535

反応式

HRID 1241535 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-91805880c0424cffb923e923189a3dfb
出典データセット
uspto-grants-2006_10
特許番号
US07115608B2

関連ノート

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