Trichloroacetic Acid → 2,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol

HRID 334433

반응식

HRID 334433 반응식
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](O)=[O:4].ClC(Cl)(Cl)C([O-])=O.[Na+].[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:30]=[CH:29][C:26](C=O)=[CH:25][CH:24]=2)[CH2:19][CH2:18]1>CN(C)C=O>[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3]([C:26]1[CH:25]=[CH:24][C:23]([N:20]2[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]2)=[CH:30][CH:29]=1)[OH:4]

참가 물질

5

반응물 3

HCID 6421Trichloroacetic AcidHCID 7365334-(4-Methylpiperazin-1-yl)benzaldehydeHCID 23681045Sodium Trichloroacetate

생성물 1

HCID 682771722,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.0 ml (10.00 mmol) of trichloroacetic acid and, in small portions, 1.854 g. (10 mmol) of sodium 2,2,2-trichloroacetate are added at room temperature to a solution of 1.362 g (6.67 mmol) of 4-(4-methylpiperazine-1-yl)benzaldehyde in 13.5 ml of dimethylformamide. The reaction mixture is stirred for 3 hours at room temperature. The solvent is concentrated and the crude reaction product extracted with ethyl acetate. The organic phase is washed using saturated sodium bicarbonate solution. The organic phases are combined, dried on magnesium sulfate and then concentrated to yield 1.760 g (yield=82%) of 2,2,2-trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol in the form of a white solid.

후처리

  1. concentrationThe solvent is concentrated
  2. customthe crude reaction product
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is washed
  5. customdried on magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-515ca87369a043708f8648e14abc16e2
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883821B2

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