Potassium Carbonate → 6-(3-Phenoxycarbonylaminopropoxy)carbostyril

HRID 1856766노트

반응식

HRID 1856766 반응식
Cl.[NH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2.C(=O)([O-])[O-].[K+].[K+].[C:24](Cl)(=[O:32])[O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>O.C(#N)C>[O:25]([C:24]([NH:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[NH:13][C:12](=[O:17])[CH:11]=[CH:10]2)=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 15891Phenyl chloroformateHCID 114141486-(3-aminopropoxy)-1H-quinolin-2-one;hydrochloride

생성물 1

HCID 221326106-(3-Phenoxycarbonylaminopropoxy)carbostyril수율 90.3%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6342Acetonitrile용매

실험 절차

To a mixture of water (50 ml) and acetonitrile (50 ml) are added 6-(3-aminopropoxy)carbostyril hydrochloride (5.0 g) and potassium carbonate (3.4 g) at room temperature. The mixture is stirred at room temperature for 2 hours, and cooled to -5° C. To the mixture is added dropwise phenyl chlorocarbonate (3.9 g) while the temperature of the mixture is kept below 0° C. The mixture is stirred at the same temperature for 1 hour, and thereto is added water (100 ml), and then the mixture is further stirred for 0.5 hour. The precipitated crystals are collected by filtration, and washed successively with water and acetone to give 6-(3-phenoxycarbonylaminopropoxy)carbostyril (6.0 g) as a white powder.

후처리

  1. temperaturecooled to -5° C
  2. customis kept below 0° C
  3. stirringThe mixture is stirred at the same temperature for 1 hour
  4. stirringthe mixture is further stirred for 0.5 hour
  5. filtrationThe precipitated crystals are collected by filtration
  6. washwashed successively with water and acetone

출처 및 근거

ORD 기록
ord-42764983a41c4be598441f4d5877af9a
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06143763

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