HRID1254279
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID81138
Methanamine, N-methoxy-, hydrochloride
C2H8ClNO
HCID81531
Diisopropylethylamine
C8H19N
HCID2755965
4-(tert-Butoxycarbonyl)morpholine-2-carboxylic acid
C10H17NO5
HCID9886157
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of (±)-4-(tert-butoxycarbonyl)morpholine-2-carboxylic acid (1.51 g, 6.53 mmol), N,O-dimethylhydroxylamine hydrochloride (0.83 g, 8.49 mmol) and i-Pr2NEt (3.1 mL, 17.6 mmol) in CH2Cl2 (30 mL) was added solid HATU (3.01 g, 7.85 mmol). The mixture was stirred at rt for 3 d, diluted with ether (175 mL), washed with 5% aq HCl (2×50 mL) and satd aq NaHCO3 (50 mL) and dried over MgSO4. Removal of the solvent left (±)-tert-butyl 2-(methoxy(methyl)carbamoyl)morpholine-4-carboxylate (1.73 g, 96%) as an oil.
WORKUP
后处理
- washwashed with 5% aq HCl (2×50 mL)
- dry with materialdried over MgSO4
- customRemoval of the solvent
- waitleft (±)-tert-butyl 2-(methoxy(methyl)carbamoyl)morpholine-4-carboxylate (1.73 g, 96%) as an oil