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

HRID 2068877ノート

反応式

HRID 2068877 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-0bbc6eb4442448a58818a924b6e086df
出典データセット
uspto-grants-2012_10
特許番号
US08299070B2

反応ノート

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