HRID2216998
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of trans-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexylamine (500 mg, 2.20 mmol) (from Example 20a supra) and triethylamine (1.52 mL, 10.90 mmol) (Aldrich) in dichloromethane (15 mL) was added a 20% phosgene in toluene solution (3.2 mL, 6.50 mmol) (Fluka) at 0° C. The resulting mixture was stirred for 15 minutes, then filtered and the filtrate was concentrated to a residue that was distilled at 110° C. under high vacuum using a Kugelrohr apparatus to give trans-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl isocyanate (485 mg) as a colorless liquid.
WORKUP
后处理
- filtrationfiltered
- concentrationthe filtrate was concentrated to a residue that
- distillationwas distilled at 110° C. under high vacuum