Trifluoroacetic acid → 1-[4-(Trifluoromethoxy)benzenesulfonyl]piperazine

HRID 506862ノート

反応式

HRID 506862 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]([F:27])([F:26])[F:25])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:27][C:24]([F:25])([F:26])[O:23][C:20]1[CH:21]=[CH:22][C:17]([S:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)(=[O:16])=[O:15])=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 458629304-(4-Trifluoromethoxy-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 20794021-[4-(Trifluoromethoxy)benzenesulfonyl]piperazine収率 87%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a cold (0 C) solution of 4-(4-trifluoromethoxy-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (1.15 g, 2.8 mmol) in DCM (3 ml) was added TFA (2 ml). The resulting solution was stirred for 1 hr. Solvent was then removed under reduced pressure. The crude solid was taken-up in AcOEt (15 ml) and washed with NaHCO3 sat (2×5 ml), water (5 ml) and finally with brine (5 ml). The organic layer was dried over MgSO4 and the solvent was removed under vacuo to yield the desired 1-(4-trifluoromethoxy-benzenesulfonyl)-piperazine as a white solid (753 mg, 87% yield).

後処理

  1. customSolvent was then removed under reduced pressure
  2. washwashed with NaHCO3
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe solvent was removed under vacuo

出典と根拠

ORDレコード
ord-9c44250bc06b4969abc709fb7e3ae94f
出典データセット
uspto-grants-2010_08
特許番号
US07786121B2

反応ノート

読み込み中…