Sodium sulfate decahydrate → (5-Amino-1-methyl-1H-indol-2-yl)methanol

HRID 239900노트

반응식

HRID 239900 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[C:6]([C:12](OCC)=[O:13])=[CH:5]2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[C:6]([CH2:12][OH:13])=[CH:5]2

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 11424506Ethyl 5-amino-1-methyl-1H-indole-2-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 45098216(5-Amino-1-methyl-1H-indol-2-yl)methanol수율 114.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of ethyl 5-amino-1-methyl-1H-indole-2-carboxylate (9.21 g) in THF (55 mL) was added dropwise to a solution of lithium aluminum hydride (2.08 g) in THF (110 mL) at 5° C., and the mixture was stirred at room temperature for 4.5 hr. To the reaction mixture was added sodium sulfate decahydrate (20.4 g), and the mixture was stirred at room temperature for 30 min. The insoluble material was filtered off and washed with THF. The filtrate was concentrated under reduced pressure to dryness to give the title compound (8.50 g, yield 100%) as a yellow solid.

후처리

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. filtrationThe insoluble material was filtered off
  3. washwashed with THF
  4. concentrationThe filtrate was concentrated under reduced pressure to dryness

출처 및 근거

ORD 기록
ord-3571420a6ef14ba59b2e2d74bb5f0d10
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642770B2

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