HRID857928

反应详情

EQUATION

反应方程式

HRID 857928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A fine suspension of 2-amino-4,6-dichloro-pyrimidine-5-carbaldehyde (3.0 g, 15 mmol); (Seela, F.; Stecker, H. Helv. Chim. Acta 1986, 69, 1602) in THF was cooled to −78° C. A 3M solution of MeMgBr in THF (25 mL, 75 mmol, 5 equiv.) was added over 3 h, keeping the internal temperature at −78° C. The mixture was stirred for a further 0.5 h, quenched with 100 ml H2O, and neutralized with aw. HCl. Extraction (EtOAc) gave 1-(2-amino-4,6-dichloro-pyrimidin-5-yl)-ethanol as a pale yellow solid (2.5 g, 76%) which was used without further purification.

WORKUP

后处理

  1. customat −78° C
  2. customquenched with 100 ml H2O
  3. extractionExtraction (EtOAc)