Acetic Acid → 3-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

HRID 503114노트

반응식

HRID 503114 반응식
[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=C(C#N)[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2.[C:21]([OH:24])(=[O:23])[CH3:22].O.S(=O)(=O)(O)O>C(OCC)(=O)C>[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=[C:22]([C:21]([OH:24])=[O:23])[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 222607323-Benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile

생성물 1

HCID 222606653-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

To 288 mg of 3-benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile were added 3 ml of glacial acetic acid, 1 ml of water and 0.8 ml of concentrated sulfuric acid, and the mixture was stirred at 110° C. for 4 hours. After standing to cool, the mixture was added with 120 ml of ethyl acetate, sequentially washed with water and brine, dried over anhydrous magnesium sulfate. After filtering the organic layer through a silica gel pat, the solvent was evaporated, to give 307 mg of the title compound as ocher yellow crystals.

후처리

  1. temperatureto cool
  2. washsequentially washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtering the organic layer through a silica gel pat
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-bbd7f2500aab4d89826c9607d4fbeb8c
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776890B2

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