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

HRID 1723825

反応式

HRID 1723825 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-d4a7a68439a7489c929028d77cf10ea9
出典データセット
uspto-grants-2009_02
特許番号
US07485644B2

関連ノート

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