Dimethylamine → N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate

HRID 477299

反応式

HRID 477299 の反応式
[CH3:1][NH:2][CH3:3].[F:4][B-:5]([F:8])([F:7])[F:6].C(O[C:12]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:13][CH:14]=[N+:15]([CH3:17])[CH3:16])C.C(OCC)C>C(Cl)Cl>[F:4][B-:5]([F:8])([F:7])[F:6].[CH3:1][N:2]([CH3:3])[C:12]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:13][CH:14]=[N+:15]([CH3:17])[CH3:16]

参加物

5

実験手順

A solution of dimethylamine (233 cc) in methylene chloride is added in the course of 1 hour 20 minutes, at a temperature of approximately 20° C., to a solution of N-(3-ethoxy-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (1,007 g) in methylene chloride. Anhydrous ethyl ether (2,000 cc) is then run slowly into the reaction medium, and the crystalline product is then separated off by filtration and dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of approximately 20° C. N-(3-Dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (925 g), m.p. 102° C., is thereby obtained.

後処理

  1. customthe crystalline product is then separated off by filtration
  2. customdried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of approximately 20° C

出典と根拠

ORDレコード
ord-6c30ed02d468450493491dda1e297617
出典データセット
uspto-grants-1989_12
特許番号
US04886835

関連ノート

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