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

HRID 334433

反応式

HRID 334433 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-515ca87369a043708f8648e14abc16e2
出典データセット
uspto-grants-2014_11
特許番号
US08883821B2

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