HRID1602664

反应详情

EQUATION

反应方程式

HRID 1602664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

##STR52## HCl gas was bubbled through a stirred suspension of 2-[6-methyl-2-oxo-3-(benzyloxycarbonylamino)-2H-pyridin-1-yl]acetic acid t-butyl ester (16-3; 12.3 g, 33 mmol) in ethyl acetate (250 ml) at -15° C. for 20 min. The resulting solution was allowed to warm to room temperature and was then stirred there for 3 h. After purging with argon, the bulk of the solvent was rotavapped off and ether added to the residue. The solid which precipitated was filtered off and washed with ether. The title compound 16-4 was thus obtained as a white fluffy powder: 1H NMR (CD3OD) δ 2.32 (s, 3 H), 4.86 (s, 2 H), 5.18 (s, 2 H), 6.24 (d, J=7.9 Hz, 1 H), 7.31-7.41 (m, 6 H), 7.94 (br s, 1 H).

WORKUP

后处理

  1. customAfter purging with argon
  2. additionether added to the residue
  3. customThe solid which precipitated
  4. filtrationwas filtered off
  5. washwashed with ether