反応 #63322

反応方程式

sodium carbonate

methanesulphonic acid

5-[(dimethylamino)methyl]-2-furanmethanol

4-aminobutanol

→

title compound

収率 29.2%

5-[(4-Aminobutoxy)methyl]-N,N-dimethyl-2-furanmethanamine

収率 29.2%

溶媒

water

tetrahydrofuran

反応条件

後処理

1. 1
   温度was heated at 100° for 11/2 h
2. 2
   ろ過the suspension was filtered
3. 3
   その他the filtrate was evaporated
4. 4
   その他to give a red oil which
5. 5
   抽出extracted with ether
6. 6
   workup.DISTILLATIONThe extract was distilled

実験手順

A mixture of methanesulphonic acid (86 g), 5-[(dimethylamino)methyl]-2-furanmethanol (15.5 g) and 4-aminobutanol (17.8 g) in dry tetrahydrofuran was heated at 100° for 11/2 h. Excess sodium carbonate was added to the cooled solution, the suspension was filtered and the filtrate was evaporated to give a red oil which was dissolved in water and extracted with ether. The extract was distilled to give the title compound as an oil (6.6 g) b.p. 100°-110°, 0.08 mm. TLC silica, methanol/ammonia 0.88 80:1, Rf 0.3.

出典