Sodium Hydroxide → 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine

HRID 2263263

反応式

HRID 2263263 の反応式
Cl.[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[S:13][CH:14]=1.[OH-].[Na+]>O>[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[S:13][CH:14]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 687762881-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride

生成物 1

HCID 687762891-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine収率 56.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 4 N solution (50 ml) of hydrogen chloride in ethyl acetate was added to a solution of tert-butyl 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate (4.20 g, 11.0 mmol) in ethyl acetate (100 ml), and the mixture was stirred at room temperature for 14 hours. Hexane was added to the reaction mixture, and crystals were collected by filtration to give 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride. The hydrochloride was dissolved in water, neutralized with a 1 N sodium hydroxide aqueous solution, and extracted with chloroform. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give 1.76 g (56.8%) of the desired product as a solid.

後処理

  1. extractionextracted with chloroform
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a0dc484bb6a1418eaf18f6d2c2bc8459
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

関連ノート

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