Sodium Hydroxide → 1-(5-Bromo-1,3-thiazol-2-yl)piperazine

HRID 1282187ノート

反応式

HRID 1282187 の反応式
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[S:11][C:12]([Br:15])=[CH:13][N:14]=2)[CH2:6][CH2:5]1)(=O)C.[OH-].[Na+]>Cl>[Br:15][C:12]1[S:11][C:10]([N:7]2[CH2:6][CH2:5][NH:4][CH2:9][CH2:8]2)=[N:14][CH:13]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18422993HCID 18422993、化合物

生成物 1

HCID 184230061-(5-Bromo-1,3-thiazol-2-yl)piperazine収率 87.7%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

4-Acetyl-1-(5-bromothiazol-2-yl)piperazine (2.0 g) was dissolved in 6N hydrochloric acid and refluxed under heating for 4.5 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 brown oil (1.5 g). The obtained brown oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1) to give the title compound (1.1 g) as a pale-yellow solid.

後処理

  1. temperaturerefluxed
  2. temperatureunder heating for 4.5 hr
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-7cb82f606874419db937c3a58d6b0fdb
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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