Water → HCID 54274887, 화합물

HRID 65574노트

반응식

HRID 65574 반응식
[CH3:1][C:2]([CH3:28])([CH:7]([NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=1)(=[O:20])=[O:19])[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=1)[C:3]([O:5][CH3:6])=[O:4].[H-].[Na+].[CH3:31]I.O>CN(C)C=O>[CH3:1][C:2]([CH3:28])([CH:7]([N:17]([CH3:31])[S:18]([C:21]1[CH:22]=[CH:23][C:24]([CH3:27])=[CH:25][CH:26]=1)(=[O:19])=[O:20])[CH2:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH3:16])=[CH:13][CH:14]=1)[C:3]([O:5][CH3:6])=[O:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 53810576HCID 53810576, 화합물

생성물 1

HCID 54274887HCID 54274887, 화합물수율 96%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A solution of 405 g of methyl 2,2-dimethyl-4-(p-methoxyphenyl)-3-(p-toluenesulphonamido)butyrate in 1800 ml of dry dimethylformamide is added to a mechanically stirred suspension of 52.8 g of sodium hydride in 320 ml of the same solvent. After the reaction mixture has been heated at 80° C. for 1 hour it is cooled when 93 ml of methyl iodide is added. After an additional period of heating (under reflux) the mixture, after being cooled, is poured into plenty of water. A white crystallisate separates. After filtration and drying it melts at 132°-134° C. Yield 96%.

후처리

  1. additionis added
  2. temperatureAfter an additional period of heating
  3. temperature(under reflux) the mixture
  4. temperatureafter being cooled
  5. filtrationAfter filtration
  6. customdrying it melts at 132°-134° C

출처 및 근거

ORD 기록
ord-514973f2c1c24851a3cc2d6ede742fab
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128548

반응 노트

불러오는 중…