Water → Flecainide

HRID 460428

반응식

HRID 460428 반응식
[F:1][C:2]([F:22])([F:21])[CH2:3][O:4][C:5]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]([F:20])([F:19])[F:18])=[CH:11][C:6]=1[C:7]([O:9]C)=O.[NH2:23][CH2:24][CH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][NH:26]1.O>C1(C)C=CC=CC=1>[CH:13]1[C:12]([O:15][CH2:16][C:17]([F:20])([F:19])[F:18])=[CH:11][C:6]([C:7]([NH:23][CH2:24][CH:25]2[NH:26][CH2:27][CH2:28][CH2:29][CH2:30]2)=[O:9])=[C:5]([O:4][CH2:3][C:2]([F:1])([F:22])[F:21])[CH:14]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 90865Piperidine-2-methylamineHCID 2727094Methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate

생성물 1

HCID 3356Flecainide수율 87.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate (1.5 g), 2-(aminomethyl)piperidine (0.62 g) in toluene (3 ml) was stirred at reflux for 10 hours. After cooling to room temperature, water (10 ml) was added and two layers solution were separated. The aqueous layer was extracted with toluene (2×10 ml) and the combined organic layers were washed with water (3×10 ml). The organic layer was concentrated under reduced pressure to give Flecainide free base as a white solid (1.63 g, 85%).

후처리

  1. temperatureat reflux for 10 hours
  2. customtwo layers solution were separated
  3. extractionThe aqueous layer was extracted with toluene (2×10 ml)
  4. washthe combined organic layers were washed with water (3×10 ml)
  5. concentrationThe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-da87f08ae68749968e27a5d0ae886fab
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196197B2

연결된 노트

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