Water → Methyl 4-{[(4-biphenylyloxy)acetyl]amino}-3-thiophenecarboxylate

HRID 14592

반응식

HRID 14592 반응식
[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][C:11](=[O:15])[CH2:12]CCl)=[CH:8][S:7][CH:6]=1)=[O:4].C(=O)([O-])[O-].[K+].[K+].[OH:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:25][CH:24]=1.O>CN(C)C=O>[CH3:1][O:2][C:3]([C:5]1[C:9]([NH:10][C:11](=[O:15])[CH2:12][O:22][C:23]2[CH:24]=[CH:25][C:26]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:27][CH:28]=2)=[CH:8][S:7][CH:6]=1)=[O:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 71034-HydroxybiphenylHCID 11430Potassium CarbonateHCID 686867214-(3-Chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester

생성물 1

HCID 24886422Methyl 4-{[(4-biphenylyloxy)acetyl]amino}-3-thiophenecarboxylate수율 101.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

To a solution of 4-(3-chloro-propionylamino)-thiophene-3-carboxylic acid methyl ester ([51486-30-7], 0.1 g, 0.43 mmol) in dimethylformamide (1.5 mL) was added potassium carbonate (0.88 g, 0.64 mmol) and 4-hydroxybiphenyl (0.087 g, 0.514 mmol) and the reaction mixture was then stirred overnight at 90° C. After such time the reaction mixture was allowed to cool to room temperature, water was added (in excess of 5 mL) leading to precipitation. The precipitate was then filtered, washed with water and dried in vacuo to yield the title compound as a white solid (0.16 g, 87%).

후처리

  1. temperatureto cool to room temperature
  2. customleading to precipitation
  3. filtrationThe precipitate was then filtered
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-d7e989d7129647f6a76d803531d83bbc
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732452B2

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