HRID2117843

反应详情

EQUATION

反应方程式

HRID 2117843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture of ethyl 2-(isobutyrylamino)-1,3-thiazole-4-carboxylate (1.4 g) and tetrahydrofuran (28 ml) was added lithium borohydride (252 mg) portionwise, and the mixture was refluxed for 6 hours. The reaction mixture was cooled to 0° C., quenched with methanol (5 ml) and concentrated in vacuo. The residue was suspended with 10% methanol/chloroform (100 ml), and the insoluble materials were filtered off. The filtrate was purified by flash column chromatography on silica-gel with 5% methanol/chloroform as an eluent. The crystalline residue was collected and washed with diisopropyl ether to give N-[4-(hydroxymethyl)-1,3-thiazol-2-yl]-2-methylpropanamide (1.0 g).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 6 hours
  2. customquenched with methanol (5 ml)
  3. concentrationconcentrated in vacuo
  4. filtrationthe insoluble materials were filtered off
  5. customThe filtrate was purified by flash column chromatography on silica-gel with 5% methanol/chloroform as an eluent
  6. customThe crystalline residue was collected
  7. washwashed with diisopropyl ether