HRID1887684
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 25 mL round bottom flask charged with tert-butyl (2-(N-methylmethylsulfonamido)pyridin-3-yl)methylcarbamate (118 mg, 0.26 mmol) was added a 40% solution of TFA in CH2Cl2 (4 mL). The resulting mixture was stirred for 20 min, then the volatiles were evaporated. Toluene (4 mL) was added to the crude followed by evaporation. This procedure was repeated once. A solution of the crude residue in CH2Cl2 (4 mL) was treated with Amberlyst A-21 (1.8 g) and stirred for 30 min. The Amberlyst A-21 resin was filtered off and washed with CH2Cl2 (20 mL). The volatiles were evaporated to yield N-(3-(aminomethyl)pyridin-2-yl)-N-methylmethanesulfonamide (50 mg, 0.23 mmol, 88%).
WORKUP
后处理
- customthe volatiles were evaporated
- additionToluene (4 mL) was added to the crude
- customfollowed by evaporation
- additionA solution of the crude residue in CH2Cl2 (4 mL) was treated with Amberlyst A-21 (1.8 g)
- stirringstirred for 30 min
- filtrationThe Amberlyst A-21 resin was filtered off
- washwashed with CH2Cl2 (20 mL)
- customThe volatiles were evaporated