HRID983448

反应详情

EQUATION

反应方程式

HRID 983448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-4-(2-chloro-pyridin-3-yl)-[1,3,5]triazine (1.7 g, 7.5 mmol) was stirred overnight at RT with 3,4,5-trimethoxyaniline (1.5 g, 8.3 mmol) in IpOH (200 mL). After addition of Et3N (2 ml), stirring was continued for an additional day. The mixture was concentrated, triturated with t-BuOMe and filtered, rinsing with a small amount of IpOH. The [4-(2-chloro-pyridin-3-yl)-[1,3,5]triazin-2-yl]-(3,4,5-trimethoxy-phenyl)amine (2.5 g) was isolated as the Et3HN+Cl− salt. Part of this material was filtered through a plug of silica and analyzed. MS m/z=374 [M+H]+; 3H). Calc'd for C17H16ClN5O3: 373.09. Remaining material was used without filtering in the next step.

WORKUP

后处理

  1. waitwas continued for an additional day
  2. concentrationThe mixture was concentrated
  3. customtriturated with t-BuOMe
  4. filtrationfiltered
  5. washrinsing with a small amount of IpOH