反应详情

Trimethylsilyl iodide (3.07 mL) was added to a dichloromethane (20 mL) solution of (3R,5R)-3-((R)-1-benzyloxyethyl)-5-(4-chlorophenyl)morpholin (1.44 g). Stirring was continued for 10 hours at room temperature. Additional trimethylsilyl iodide (3.07 mL) was added, and the resultant was stirred at room temperature for 4 days. Additional trimethylsilyl iodide (3.07 mL) was further added, and stirring was continued for 1 day. Additional trimethylsilyl iodide (3.07 mL) was further added, and stirring was continued for 10 hours at room temperature. A 5 N sodium hydroxide solution was added, and the organic layer was partitioned. The organic layer was dried over anhydrous magnesium sulfate. The resultant was purified with silica gel column chromatography (heptane/ethyl acetate). The title compound (903 mg) was obtained. The physical property values are as follows.

1. stirringthe resultant was stirred at room temperature for 4 days
2. stirringstirring
3. waitwas continued for 1 day
4. stirringstirring
5. waitwas continued for 10 hours at room temperature
6. customthe organic layer was partitioned
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. customThe resultant was purified with silica gel column chromatography (heptane/ethyl acetate)