反応 #2383797

反応方程式

2-[(2-fluoro-5-nitrobenzyl)(isopropyl)amino]ethanol

sodium hydroxide

→

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

溶媒

water

DMSO

反応条件

後処理

1. 1
   ろ過the solids were collected by filtration
2. 2
   抽出The filtrate was extracted with methylene chloride (3×150 ml)
3. 3
   洗浄washed with water
4. 4
   乾燥dried with magnesium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮concentrated to an oil
7. 7
   workup.DISSOLUTIONThe solid and the oil were dissolved in hot 95% ethanol
8. 8
   温度cooled
9. 9
   ろ過The solids were collected by filtration (17.47 g, 68%), MS m/z 237 [M+H]+

実験手順

To 2-[(2-fluoro-5-nitrobenzyl)(isopropyl)amino]ethanol (31.2 g, 90 mmol) in DMSO (250 ml) was added 25% sodium hydroxide solution (43.2 g, 270 mmol) and the mixture was allowed to stir for 3 h. The reaction was diluted to twice its volume with water and the solids were collected by filtration. The filtrate was extracted with methylene chloride (3×150 ml), washed with water, dried with magnesium sulfate, filtered, and concentrated to an oil. The solid and the oil were dissolved in hot 95% ethanol, then cooled. The solids were collected by filtration (17.47 g, 68%), MS m/z 237 [M+H]+.

出典