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

HRID 239900ノート

反応式

HRID 239900 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3571420a6ef14ba59b2e2d74bb5f0d10
出典データセット
uspto-grants-2014_02
特許番号
US08642770B2

反応ノート

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