Water → HCID 13606280, 화합물

HRID 2309244노트

반응식

HRID 2309244 반응식
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]([C:6]([NH:8][CH:9]([CH2:13][CH:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][C:15]2=[O:23])[C:10]([OH:12])=[O:11])=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].[CH3:28]I.O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([NH:8][CH:9]([CH2:13][CH:14]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:16]([CH3:28])[C:15]2=[O:23])[C:10]([OH:12])=[O:11])=[O:7])=[CH:24][CH:25]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 13393254HCID 13393254, 화합물

생성물 1

HCID 13606280HCID 13606280, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

479 Milligrams of 2-(4-chlorobenzoylamino)-3-(oxindol-3-yl)propionic acid 1/4-hydrate prepared in Example 3 and 70 mg of 50% sodium hydride (in oil) were admixed in 5 ml of dimethylformamide, and the mixture was stirred at a room temperature for 1 hour. Then a solution containing 0.23 g of methyl iodide in 3 ml of dimethylformamide was added dropwise gradually to the mixture, and the whole reaction mixture was stirred at a room temperature for 4 hours. The reaction mixture was poured into a large volume of water, and the organic material was extracted with chloroform, then the chloroform layer was washed with water and dried. Chloroform was removed by evaporation to yield 125 mg of 2-(4-chlorobenzoylamino)-3-(1-methyloxindol-3-yl)propionic acid.

후처리

  1. additionwas added dropwise gradually to the mixture
  2. customthe whole reaction mixture
  3. stirringwas stirred at a room temperature for 4 hours
  4. extractionthe organic material was extracted with chloroform
  5. washthe chloroform layer was washed with water
  6. customdried
  7. customChloroform was removed by evaporation

출처 및 근거

ORD 기록
ord-a6b049a51f414cc1896eb629103a1e0c
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04694017

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