HRID1854559

反应详情

EQUATION

反应方程式

HRID 1854559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationFilter the mixture
  2. washwash the filter cake with isopropyl acetate (2.5 L)
  3. customdry on the
  4. filtrationfilter for 30 minutes