Sodium hydride → HCID 13913551、化合物

HRID 330004ノート

反応式

HRID 330004 の反応式
[SH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].Cl[CH:15]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[Cl:29])[CH2:16][N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1>CN(C)C=O>[Cl:29][C:23]1[CH:24]=[C:25]([Cl:28])[CH:26]=[CH:27][C:22]=1[CH:15]([S:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][CH:11]=1)[CH2:16][N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 237573Methyl 4-sulfanylbenzoateHCID 124607821-[2-Chloro-2-(2,4-dichlorophenyl)ethyl]-1H-imidazole

生成物 1

HCID 13913551HCID 13913551、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

415 mg of methyl 4-mercaptobenzoate were dissolved in 3 ml of dry dimethylformamide, and 108 mg of a 55% w/w suspension of sodium hydride in mineral oil were then added to the resulting solution, whilst ice-cooling, after which the mixture was stirred at room temperature for 30 minutes. 567 mg of a solution of 1-[2-chloro-2-(2,4-dichlorophenyl)ethyl]imidazole dissolved in 3 ml of dry dimethylformamide were then added to the resulting solution, and the mixture was heated at 60° to 70° C. for 7 hours. At the end of this time, the resulting mixture was treated and purified similarly to the procedure described in Example 1, to give 317 mg of the title compound as colorless crystals, melting at 121°-124° C.

後処理

  1. additionwere then added to the resulting solution, whilst ice-
  2. temperaturecooling
  3. additionwere then added to the resulting solution
  4. temperaturethe mixture was heated at 60° to 70° C. for 7 hours
  5. additionAt the end of this time, the resulting mixture was treated
  6. custompurified similarly to the procedure

出典と根拠

ORDレコード
ord-50ca0ba7a3994603866fccc856d122b4
出典データセット
uspto-grants-1990_01
特許番号
US04894385

反応ノート

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