反応 #2383802

反応方程式

sodium hydroxide

7-nitro-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

formaldehyde

formic acid

→

solid

収率 61.5%

4-Methyl-7-nitro-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

収率 61.5%

溶媒

water

反応条件

後処理

1. 1
   温度cooled

実験手順

A mixture of 7-nitro-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (11.53 g, 50 mmol), 37% formaldehyde (25 ml, 335 mmol) and 88% formic acid (15 ml, 340 mmol) was heated at 80° C. for 24 h, cooled and poured into water (150 ml). The suspension was Is basified with 25% aqueous sodium hydroxide to give a brown solid (7.52 g). The aqueous layer was extracted with methylene chloride (3×200 ml), washed with saturated brine solution, and dried over magnesium sulphate to give yellow crystals (1.02 g). This sample was combined with the solid obtained earlier and suspended in isopropanol (750 ml), refluxed for several hours and then filtered. The filtrate was acidified to give the title compound (9.51 g).

出典