反应 #1519151

ord-b18b09b29376467195a0b48d17f1224b

反应方程式

[H-].[Na+]
sodium hydride
CC(C)(C)OC(=O)NC1CCN([C@@H]2c3ccccc3OC[C@H]2OCc2cc(Br)cc(Br)c2)CC1
compound
CC(C)(C)OC(=O)NC1CCN([C@@H]2c3ccccc3OC[C@H]2OCc2cc(Br)cc(Br)c2)CC1
tert-Butyl trans-1-{3-[(3,5-dibromobenzyl)oxy]-3,4-dihydro-2H-chromen-4-yl}-4-piperidylcarbamate
CI
methyl iodide
CN(C(=O)OC(C)(C)C)C1CCN([C@@H]2c3ccccc3OC[C@H]2OCc2cc(Br)cc(Br)c2)CC1
expected product
CN(C(=O)OC(C)(C)C)C1CCN([C@@H]2c3ccccc3OC[C@H]2OCc2cc(Br)cc(Br)c2)CC1
tert-Butyl trans-1-{3-[(3,5-dibromobenzyl)oxy]-3,4-dihydro-2H-chromen-4-yl}-N-methyl-4-piperidylcarbamate

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with ethyl acetate

实验过程

0.2 g of sodium hydride (60% in oil) is added to 1 g of the compound obtained in Step B of Example 9 and 0.42 ml of methyl iodide in 10 ml of tetrahydrofuran, maintaining the temperature of the reaction mixture at 0° C. After 15 minutes at that temperature, the mixture is stirred for 48 hours at ambient temperature, diluted with water and extracted with ethyl acetate. After conventional treatment, the expected product is isolated.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07612061B2uspto-grants-2009_11