1H-Indazole-4-carboxylic acid, 1-acetyl-6-bromo-, methyl ester → methyl 6-bromo-1H-indazole-4-carboxylate

HRID 1854104노트

반응식

HRID 1854104 반응식
C([N:4]1[C:12]2[CH:11]=[C:10]([Br:13])[CH:9]=[C:8]([C:14]([O:16][CH3:17])=[O:15])[C:7]=2[CH:6]=[N:5]1)(=O)C>CO.Cl>[Br:13][C:10]1[CH:9]=[C:8]([C:14]([O:16][CH3:17])=[O:15])[C:7]2[CH:6]=[N:5][NH:4][C:12]=2[CH:11]=1

참가 물질

4

반응물 1

HCID 682954331H-Indazole-4-carboxylic acid, 1-acetyl-6-bromo-, methyl ester

생성물 1

HCID 24728062methyl 6-bromo-1H-indazole-4-carboxylate수율 71.7%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

To a stirred solution of methyl 1-acetyl-6-bromo-1H-indazole-4-carboxylate (18 g, 61.0 mmol) in methanol (350 mL), 6N HCl (350 mL) was added and stirred it at 60° C. for 8 h. On completion of reaction, solvent was removed under reduced pressure then basified with saturated NaHCO3 solution till pH 8. The solid precipitate was filtered and dried under vacuum before being stirred in diethyl ether for 15 min, filtered and dried to afford methyl 6-bromo-1H-indazole-4-carboxylate (11 g, 71.7%).

후처리

  1. customOn completion of reaction, solvent
  2. customwas removed under reduced pressure
  3. filtrationThe solid precipitate was filtered
  4. customdried under vacuum
  5. stirringbefore being stirred in diethyl ether for 15 min
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-b0bb07ce6cf44fca83cba7d8f1a82ace
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962620B2

반응 노트

불러오는 중…