HRID1854559
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
Add hydrogen chloride (267.24 g, 1.02 mol, 4M in 1,4-dioxane) to (1S,3R)-5-bromo-3-({[tert-butyl(dimethyl)silyl]oxy}methyl)-1-methyl-1,2,3,4-tetrahydroisoquinoline (419 g, 1.02 mol) in isopropyl acetate (4.19 L) at 10° C. and stir for 15 minutes in an appropriate vessel. Filter the mixture and wash the filter cake with isopropyl acetate (2.5 L), dry on the filter for 30 minutes, then under vacuum in an oven at 40° C. for 16 hours to give the title compound (380 g, 0.89 mol). MS (m/z): 370(M-Cl (79Br)), 372(M-Cl (81Br)).
WORKUP
后处理
- filtrationFilter the mixture
- washwash the filter cake with isopropyl acetate (2.5 L)
- customdry on the
- filtrationfilter for 30 minutes