ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → HCID 21108202、化合物

HRID 1766006
ノート
印刷プレビュー

反応式

HRID 1766006 の反応式
[BH4-].[Na+].[C:3]([N:6]1[C:14]2[C:9](=[CH:10][C:11]([C:15](=[O:21])[CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])=[CH:12][CH:13]=2)[CH2:8][CH2:7]1)(=[O:5])[CH3:4].O>CO>[C:3]([N:6]1[C:14]2[C:9](=[CH:10][C:11]([CH:15]([OH:21])[CH2:16][CH2:17][N:18]([CH3:19])[CH3:20])=[CH:12][CH:13]=2)[CH2:8][CH2:7]1)(=[O:5])[CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 17848792HCID 17848792、化合物

生成物 1

HCID 21108202HCID 21108202、化合物収率 76.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
2.5 °C

実験手順

Sodium borohydride (0.75 g) was added to a solution of 1-(1-acetyl-2,3-dihydro-1H-indol-5-yl)-3-(dimethylamino)-1-propanone (4.3 g) obtained in Reference Example 12 in methanol (40 ml) under cooling with ice-bath, and the mixture was stirred at 0 to 5° C. for 30 minutes. After iced water was added to the reaction solution, the solvent was distilled away under reduced pressure, and the residues were extracted with ethyl acetate. The extract was washed with a saturated saline solution and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. The resultant residues were purified by alumina column chromatography (developing solvent; ethyl acetate), whereby 3-[1-acetyl-2,3-dihydro-1H-indol-5-yl]-3-hydroxy-N,N-dimethyl-1-propanamine (3.3 g) was obtained as colorless powder.

後処理

  1. temperatureunder cooling with ice-bath
  2. distillationthe solvent was distilled away under reduced pressure
  3. extractionthe residues were extracted with ethyl acetate
  4. washThe extract was washed with a saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled away under reduced pressure
  7. customThe resultant residues were purified by alumina column chromatography (developing solvent; ethyl acetate)

出典と根拠

ORDレコード
ord-a2eaba021c634cf892dd576950d6feaa
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07229986B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート