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

HRID 506862노트

반응식

HRID 506862 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9c44250bc06b4969abc709fb7e3ae94f
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786121B2

반응 노트

불러오는 중…