Water → Flecainide

HRID 460428

反応式

HRID 460428 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 3356Flecainide収率 87.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-da87f08ae68749968e27a5d0ae886fab
出典データセット
uspto-grants-2007_03
特許番号
US07196197B2

関連ノート

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