HRID1798311

反应详情

EQUATION

反应方程式

HRID 1798311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

Into a 50-mL round-bottom flask was placed a solution of ethyl 2-(1-hydroxy-4-methyl-6-(5-nitro-1,3,4-thiadiazol-2-yloxy)-1,3-dihydrobenzo[c][1,2]oxaborol-3-yl)propanoate (500 mg, 1.15 mmol, 1.00 equiv, 90%) in ethanol/H2O (15/5 mL). This was followed by the addition of Fe (280 mg, 5.00 mmol, 4.00 equiv). Then added 2 drops of HCl. The resulting solution was stirred for 2 h at 85° C. The reaction mixture was cooled and filtered. The filtrate was concentrated under vacuum. This resulted in 0.8 g (90%) of ethyl 2-(6-(5-amino-1,3,4-thiadiazol-2-yloxy)-1-hydroxy-4-methyl-1,3-dihydrobenzo[c][1,2]oxaborol-3-yl)propanoate as a brown solid.

WORKUP

后处理

  1. customInto a 50-mL round-bottom flask was placed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under vacuum
  5. customThis resulted in 0.8 g (90%) of ethyl 2-(6-(5-amino-1,3,4-thiadiazol-2-yloxy)-1-hydroxy-4-methyl-1,3-dihydrobenzo[c][1,2]oxaborol-3-yl)propanoate as a brown solid