Potassium Carbonate → 6-(3-Phenoxycarbonylaminopropoxy)carbostyril

HRID 1856766ノート

反応式

HRID 1856766 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 221326106-(3-Phenoxycarbonylaminopropoxy)carbostyril収率 90.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-42764983a41c4be598441f4d5877af9a
出典データセット
uspto-grants-2000_11
特許番号
US06143763

反応ノート

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