HRID1504843
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 methyl 3-{[(benzyloxy)carbonyl]amino}-N-(tert-butoxycarbonyl)alaninate (80 g, 230 mmol) in THF (800 mL) was added lithium borohydride (20 g, 920 mmol) at 0° C. The reaction mixture was allowed to warm to room temperature. After 1 hour, the reaction mixture was diluted with water and filtered. The filtrate was concentrated under reduced pressure to give benzyl tert-butyl (3-hydroxypropane-1,2-diyl)biscarbamate. MS ESI calc'd. for C16H25N2O5 [M+H]+ 325. found 325. 1H NMR (400 MHz, CDCl3) δ 7.38-7.35 (m, 5H), 5.11 (s, 2H), 4.70 (s, 1H), 4.13-4.11 (m, 1H), 3.66-3.28 (m, 4H), 2.04 (s, 2H), 1.43 (s, 9H).
WORKUP
后处理
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure