Trifluoroacetic acid → 1-[4-(2,2,2-Trifluoroethoxy)phenyl]piperazine

HRID 1723825

반응식

HRID 1723825 반응식
[F:1][C:2]([F:25])([F:24])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]2)=[CH:7][CH:6]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:25][C:2]([F:1])([F:24])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:9][CH:10]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68847847Tert-butyl 4-[4-(2,2,2-trifluoroethoxy)phenyl]piperazine-1-carboxylate

생성물 1

HCID 435103441-[4-(2,2,2-Trifluoroethoxy)phenyl]piperazine수율 91%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Crude tert-butyl 4-[4-(2,2,2-trifluoroethoxy)phenyl]piperazine-1-carboxylate (32.47 g, approx 57 mmol) was dissolved in DCM (300 ml) and TFA (69 mL) was added. The reaction was stirred at room temperature overnight then evaporated to dryness, azeotroping with toluene. The residue was partitioned between DCM and saturated sodium bicarbonate solution. The organic phase was separated, dried (MgSO4), filtered and concentrated to yield 1-[4-(2,2,2-trifluoroethoxy)phenyl]piperazine as a solid (13.48 g, 91%)

후처리

  1. customthen evaporated to dryness
  2. customazeotroping with toluene
  3. customThe residue was partitioned between DCM and saturated sodium bicarbonate solution
  4. customThe organic phase was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d4a7a68439a7489c929028d77cf10ea9
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07485644B2

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