Trifluoroacetic acid → (R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate

HRID 80755ノート

反応式

HRID 80755 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[C@H:6]([CH3:17])[CH2:5]1)(=[O:3])[CH3:2].[C:18]([OH:24])([C:20]([F:23])([F:22])[F:21])=[O:19]>C(Cl)Cl>[F:21][C:20]([F:23])([F:22])[C:18]([OH:24])=[O:19].[CH3:17][C@H:6]1[NH:7][CH2:8][CH2:9][N:4]([C:1](=[O:3])[CH3:2])[CH2:5]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86690247HCID 86690247、化合物

生成物 1

HCID 86690248(R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate収率 137.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of (R)-tert-butyl 4-acetyl-2-methylpiperazine-1-carboxylate (1.34 g, 5.53 mmol) and TFA (10 mL, 130 mmol) in DCM (30 mL) was stirred at rt for 45 min, then concentrated, diluted with DCM, and then concentrated again which was repeated 3 times. Dried under high vacuum at 80° C. to give (R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate (1.95 g). MS (ESI+) m/z 143.0 (M+H)+.

後処理

  1. concentrationconcentrated
  2. additiondiluted with DCM
  3. concentrationconcentrated again which
  4. customDried under high vacuum at 80° C.

出典と根拠

ORDレコード
ord-70d07e067fa340f483a5e47aede96369
出典データセット
uspto-grants-2014_09
特許番号
US08846656B2

反応ノート

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