Sodium Hydroxide → HCID 18422993、化合物

HRID 1282186ノート

反応式

HRID 1282186 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[S:11][CH:12]=[CH:13][N:14]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Br:15]N1C(=O)CCC1=O.[OH-].[Na+]>C(O)(=O)C>[C:1]([N:4]1[CH2:5][CH2:6][N:7]([C:10]2[S:11][C:12]([Br:15])=[CH:13][N:14]=2)[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 67184N-bromobutanimideHCID 18423162HCID 18423162、化合物

生成物 1

HCID 18422993HCID 18422993、化合物収率 68.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 4-acetyl-1-(thiazol-2-yl)piperazine (3.1 g) and N-bromosuccinimide (2.9 g) in acetic acid (14 ml) was stirred at room temperature for 1 hr. The reaction mixture was neutralized with 1N aqueous sodium hydroxide solution and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a pale-brown solid (2.9 g). The obtained pale-brown solid was purified by silica gel column chromatography (developing solvent; chloroform:methanol=20:1) to give the title compound (2.1 g) as a pale-brown solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-03f1bb9463d64664841c15e5acdee4b6
出典データセット
uspto-grants-2002_09
特許番号
US06455528B1

反応ノート

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