Hydrochloric Acid → methyl 2-(6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazol-3-yl)indole-6-carboxylate

HRID 2068877노트

반응식

HRID 2068877 반응식
C(OC([N:8]1[C:16]2[CH2:15][C:14]([CH3:18])([CH3:17])[CH2:13][CH2:12][C:11]=2[C:10]([C:19]2[N:20](C(OC(C)(C)C)=O)[C:21]3[C:26]([CH:27]=2)=[CH:25][CH:24]=[C:23]([C:28]([O:30][CH3:31])=[O:29])[CH:22]=3)=[N:9]1)=O)(C)(C)C.CO.[OH-].[Na+].Cl>O1CCCC1>[CH3:17][C:14]1([CH3:18])[CH2:15][C:16]2[NH:8][N:9]=[C:10]([C:19]3[NH:20][C:21]4[C:26]([CH:27]=3)=[CH:25][CH:24]=[C:23]([C:28]([O:30][CH3:31])=[O:29])[CH:22]=4)[C:11]=2[CH2:12][CH2:13]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 585501461-tert-butyl 6-methyl 2-(1-tert-butoxycarbonyl-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazol-3-yl)indole-1,6-dicarboxylate

생성물 1

HCID 136127476methyl 2-(6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazol-3-yl)indole-6-carboxylate수율 97%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-tert-butyl 6-methyl 2-(1-tert-butoxycarbonyl-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazol-3-yl)indole-1,6-dicarboxylate (39 g, 75 mmol) in a mixed solvent of methanol (180 ml) and tetrahydrofuran (120 ml) was added dropwise 2 N aqueous sodium hydroxide solution (149 ml, 298 mmol) under ice-cooling over 15 min, and the mixture was stirred for 15 min. Then, 1 N hydrochloric acid was added dropwise to adjust the pH to 5. The precipitated crystals were collected by filtration, washed with water, and dried under reduced pressure to give the title compound (23 g, yield 97%).

후처리

  1. temperaturecooling over 15 min
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed with water
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-0bbc6eb4442448a58818a924b6e086df
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299070B2

반응 노트

불러오는 중…