反应 #1509656

ord-0508444e6b154687afee9960963583ee

反应方程式

O
Water
[H-].[Na+]
sodium hydride
Clc1nc(Cl)c2nc[nH]c2n1
2,6-dichloro-9H-purine
CC(C)I
2-iodopropane
CC(C)n1cnc2c(Cl)nc(Cl)nc21
title compound
CC(C)n1cnc2c(Cl)nc(Cl)nc21
2,6-dichloro-9-isopropyl-9H-purine

溶剂

反应条件

温度
10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe mixture was stirred at rt for 24 hr
  2. 2
    其他the resulting solid precipitate was collected
  3. 3
    洗涤washed with water (500 ml) and heptane (2×2.5 L)
  4. 4
    其他The crude solid was crystallized from isopropyl acetate (2.1 L)

实验过程

To 2,6-dichloro-9H-purine (a) (998 g, 5.28 mol) dissolved in anhydrous DMF (5.0 L) was added sodium hydride (60% dispersion, 254 g, 6.35 mol) with stirring at 10° C. over 1 hr. 2-iodopropane (1595 g) was added and the mixture was stirred at rt for 24 hr. Water (5.0 L) was added, and the resulting solid precipitate was collected and washed with water (500 ml) and heptane (2×2.5 L). The crude solid was crystallized from isopropyl acetate (2.1 L) to provide the title compound as a solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08927281B2uspto-grants-2015_01