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Water → HCID 131714980, 화합물

HRID 1731984
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HRID 1731984 반응식
Cl[C:2]1[N:3]([C:11]2[CH:16]=[C:15]([OH:17])[C:14]([Cl:18])=[CH:13][C:12]=2[F:19])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.C(=O)([O-])[O-].[K+].[K+].Br[CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29].O>CN(C)C=O>[Cl:18][C:14]1[C:15]([O:17][CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:16][C:11]([N:3]2[CH:2]=[C:10]3[C:5]([CH2:6][CH2:7][CH2:8][CH2:9]3)=[N:4]2)=[C:12]([F:19])[CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 1850782-Chloro-5-(3-chloro-4,5,6,7-tetrahydroindazol-2-yl)-4-fluorophenol

생성물 1

HCID 131714980HCID 131714980, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

Into a solution of 3-chloro-2-(4-chloro-2-fluoro-5-hydroxyphenyl)-4,5,6,7-tetrahydro-2H-indazole (30 mg) in dimethylformamide (1 ml), there were added potassium carbonate (10 mg) and ethyl bromoacetate (20 mg), and the mixture was stirred at 80° C. for 3 hours. After cooling, water was added to the reaction mixture, followed by extraction with ether. The ether layer was washed with water twice, dried and concentrated. The residue was purified by thin layer chromatography to give 1.8 mg of 3-chloro-2-(4-chloro-2-fluoro-5-ethoxycarbonylmethoxyphenyl-4,5,6,7-tetrahydro-2H-indazole (Compound No. 1) as a glassy substance.

후처리

  1. temperatureAfter cooling
  2. extractionfollowed by extraction with ether
  3. washThe ether layer was washed with water twice
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-5cd4404395df4fb1bb8744a86b4ab362
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04624699

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