HRID1738773
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID7972
4-Methylmorpholine
C5H11NO
HCID75771
1-Hydroxybenzotriazole
C6H5N3O
HCID81138
Methanamine, N-methoxy-, hydrochloride
C2H8ClNO
HCID85083
1,2-Pyrrolidinedicarboxylic acid, 1-(1,1-dimethylethyl) ester, (2S)-
C10H17NO4
HCID2723939
1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride
C8H18ClN3
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 30 g Boc-proline and 13.6 g N,O-dimethylhydroxylamine hydrochloride in 250 ml of dichloromethane was added 26.73 g 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride, 18.83 g N-hydroxy-benzotriazol and 49.34 g N-methyl-morpholine at 0° C. The mixture was stirred overnight at room temperature. The reaction mixture was washed sequentially with saturated sodium bicarbonate, a 5% aqueous solution of citric acid and brine. The organic phase was dried over sodium sulfate. After filtration, the solvent was removed in vacuo to give 22.9 g N-methyl-N-methoxy-(Boc-proline)-amide.
WORKUP
后处理
- washThe reaction mixture was washed sequentially with saturated sodium bicarbonate
- dry with materialThe organic phase was dried over sodium sulfate
- filtrationAfter filtration
- customthe solvent was removed in vacuo