Sodium Hydroxide → 2-Methyl-4-morpholino-5-fluoroindole

HRID 1583609

反応式

HRID 1583609 の反応式
[CH3:1][C:2]1[NH:3][C:4]2[C:9]([CH:10]=1)=[C:8]([N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[C:7]([F:17])=[CH:6][C:5]=2Br.[OH-].[Na+].[H][H]>C(O)C.[C].[Pd]>[CH3:1][C:2]1[NH:3][C:4]2[C:9]([CH:10]=1)=[C:8]([N:11]1[CH2:12][CH2:13][O:14][CH2:15][CH2:16]1)[C:7]([F:17])=[CH:6][CH:5]=2

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 202589932-Methyl-4-morpholino-5-fluoro-7-bromoindoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 202589922-Methyl-4-morpholino-5-fluoroindole収率 65.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

To a solution of 24 g of 2-methyl-4-morpholino-5-fluoro-7-bromoindole in 200 ml of ethanol was added 1 of palladium-carbon and then 15 ml of a 20% aqueous sodium hydroxide solution. This mixture was subjected to catalytic reduction at room temperature and at atmospheric pressure. The reaction was stopped when a theoretical amount (about 1.7 l) of hydrogen was absorbed, and the catalyst was removed by filtration followed by concentration. The residue was purified through silica gel column chromatography (Wako gel C-200; eluent: chloroform: n-hexane=5:1) to give 11.8 g of 2-methyl-4-morpholino-5-fluoroindole.

後処理

  1. customwas subjected to catalytic reduction at room temperature and at atmospheric pressure
  2. customwas absorbed
  3. customthe catalyst was removed by filtration
  4. concentrationfollowed by concentration
  5. customThe residue was purified through silica gel column chromatography (Wako gel C-200; eluent: chloroform: n-hexane=5:1)

出典と根拠

ORDレコード
ord-110946cf9fee45b9a08952e576d6f158
出典データセット
uspto-grants-1985_11
特許番号
US04552879

関連ノート

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