Sodium hydride → HCID 13913551, 화합물

HRID 330004노트

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HRID 330004 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 13913551HCID 13913551, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50ca0ba7a3994603866fccc856d122b4
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894385

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