反应 #1178479

反应方程式

3-Methanesulfonyloxy-1-benzhydrylazetidine

cis-2,6-dimethylmorpholine

IPA

dioxane

→

title compound

收率 65.0%

Cis-4-(1-benzhydryl-3-azetidinyl)-2,6-dimethylmorpholine

收率 65.0%

溶剂

ethyl acetate

brine

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.WAITThe mixture was left
3. 3
   workup.ADDITIONwas added
4. 4
   其他The mixture was partitioned
5. 5
   洗涤The obtained organic layer was washed with saturated brine
6. 6
   干燥subsequently dried over anhydrous sodium sulfate
7. 7
   浓缩concentrated
8. 8
   其他The residue was purified by column chromatography

实验过程

3-Methanesulfonyloxy-1-benzhydrylazetidine (3.84 g, 12.1 mmol) and cis-2,6-dimethylmorpholine (6.97 mL, 60.5 mmol) were introduced into a screw vial, and IPA (10 mL) and dioxane (3 mL) were added thereto. The mixture was left to stand for 4 hours at 100° C. The reaction liquor was diluted with ethyl acetate, and saturated brine was added thereto. The mixture was partitioned. The obtained organic layer was washed with saturated brine, subsequently dried over anhydrous sodium sulfate, and then concentrated. The residue was purified by column chromatography using silica gel (Flash Chromatography System from Biotage AB, column size: 40M, hexane/ethyl acetate=9:1 to 1:1), to obtain the title compound (2.63 g, 65%) as an oily matter.

来源