HRID364426

反应详情

EQUATION

反应方程式

HRID 364426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4.5 g (0.015 mole) of 2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrochloride in 15 ml of methanol was added 40 ml of dimethylamine. The flask was sealed tightly and left standing at room temperature for 8 days. The methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm). The residue was taken up in 150 ml of chloroform, washed with 2×50 ml dil aqueous sodium hydroxide, dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation (70° C.; 30 mm). The syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which afforded 3.5 g (67%) of white crystals, m.p. 188°-90° C.

WORKUP

后处理

  1. customThe flask was sealed tightly
  2. waitleft
  3. customThe methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm)
  4. washwashed with 2×50 ml dil aqueous sodium hydroxide
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by rotary evaporation (70° C.; 30 mm)
  8. additionThe syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which