HRID323878

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID962

Water

H2O

HCID11430

Potassium Carbonate

CK2O3

HCID90290

tert-Butyl 2-bromo-2-methylpropionate

C8H15BrO2

$结构：CCOC(=O)/C(=N\O)c1csc(N)n1$

HCID6401018

Ethyl (αZ)-2-amino-α-(hydroxyimino)-4-thiazoleacetate

C7H9N3O3S

PRODUCTS

生成物

$结构：CCOC(=O)/C(=N\OC(C)(C)C(=O)OC(C)(C)C)c1csc(N)n1$

HCID6242376

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度: 42.5 °C

PROCEDURE

实验过程

Ethyl (Z)-2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetate (32.25 g) of Formula (I) is dissolved in N,N-dimethylformamide (258 ml) at room temperature. Tert.-butyl 2-bromoisobutyrate (38.47 g) and anhydrous potassium carbonate (47.61 g) are added and the resulting suspension is heated to 40-45° C. for 20-25 hrs. The reaction mass is cooled to 30-32° C. and it is added slowly to water. The resulting slurry is stirred at 25-30° C. for about one and a half hours. The product is filtered, washed with water and dried under reduced pressure. Yield: 50 g (93.37%), water content <1.0% w/w; Chromatographic purity (HPLC) >98%.

WORKUP

后处理

temperatureThe reaction mass is cooled to 30-32° C.
filtrationThe product is filtered
washwashed with water
customdried under reduced pressure