HRID704249

反应详情

EQUATION

反应方程式

HRID 704249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A 3.5N acetone solution (2.24 cc) of hydrochloric acid is added dropwise to an acetone solution (11 cc) of 10-[(2RS)-1-diethylamino-2-propyl]-N-[(2RS)-2-methylbutyl]-2-phenothiazinecarboxamidine (1.11 g). The mixture is stirred for 3 hours at 25° C. and then concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C. The residue is taken up in ethyl ether (50 cc) and the suspension is kept stirred for 3 hours at 25° C. The solid is filtered off on sintered glass, washed with ethyl ether (2×5 cc) and dried for 12 hours under reduced pressure (5 mm Hg; 0.7 kPa) to give 10-[(2RS)-1-diethylamino-2-propyl]-N-[(2RS)-2-methylbutyl]-2-phenothiazinecarboxamidine dihydrochloride (1.07 g), m.p. 212°-214° C.

WORKUP

后处理

  1. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C
  2. stirringthe suspension is kept stirred for 3 hours at 25° C
  3. filtrationThe solid is filtered off on sintered glass
  4. washwashed with ethyl ether (2×5 cc)
  5. customdried for 12 hours under reduced pressure (5 mm Hg; 0.7 kPa)