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

HRID 80755노트

반응식

HRID 80755 반응식
[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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86690247HCID 86690247, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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)+.

후처리

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

출처 및 근거

ORD 기록
ord-70d07e067fa340f483a5e47aede96369
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846656B2

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