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Water → HCID 23153447、化合物

HRID 1712641
ノート
印刷プレビュー

反応式

HRID 1712641 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[N:7]1([C:11](=O)[CH2:12][N:13]2[CH2:18][CH2:17][N:16]([C:19](=O)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14]2)[CH2:10][CH2:9][CH2:8]1.O.[OH-].[Na+]>O1CCCC1>[N:7]1([CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][N:16]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:17][CH2:18]2)[CH2:8][CH2:9][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 23153146HCID 23153146、化合物

生成物 1

HCID 23153447HCID 23153447、化合物収率 104.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Lithium aluminium hydride (405 mg) was suspended in tetrahydrofuran (10 ml) under a nitrogen atmosphere with stirring in an ice water bath, 1-(azetidin-1-yl)-2-(4-benzoylpiperazin-1-yl)ethanone (730 mg) and tetrahydrofuran (5 ml×3) was added thereto. The reaction mixture was stirred at 60° C. for 3 hours. The reaction mixture was allowed to cool down to room temperature, and water (0.4 ml), a 5N aqueous solution of sodium hydroxide (0.4 ml) and water (1.2 ml) were added thereto, followed by stirring for 13 hours. The insoluble matter in the reaction mixture was removed by filtration through celite, and washed with ethyl acetate (100 ml). The solvent was distilled off under reduced pressure to give a crude product of the title compound (687 mg) as a pale yellow oil.

後処理

  1. stirringThe reaction mixture was stirred at 60° C. for 3 hours
  2. stirringby stirring for 13 hours
  3. customThe insoluble matter in the reaction mixture was removed by filtration through celite
  4. washwashed with ethyl acetate (100 ml)
  5. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b11572b74b2f4483b041f0f82cfa2fcc
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07790885B2

反応ノート

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