反应详情

A stirred mixture of 32.1 g of (4-hydroxy-2-pyrimidinylthio)acetic acid, ethyl ester and 22.4 g of N,N-diethylaniline in 400 ml. of phosphorus oxychloride were heated under reflux for 5 hr. The phosphorus oxychloride was removed in a rotary evaporator in vacuo. The residue was poured onto ice and the mixture was extracted with 1 liter of ether. The ether solution was dried over MgSO4 and then filtered. The filtrate was taken to dryness in a rotary evaporator yielding 22.9 g of (4-chloro-2-pyrimidinylthio)acetic acid, ethyl ester (an oil). This material was used directly in the next step without purification.

1. temperatureunder reflux for 5 hr
2. customThe phosphorus oxychloride was removed in a rotary evaporator in vacuo
3. additionThe residue was poured onto ice
4. extractionthe mixture was extracted with 1 liter of ether
5. dry with materialThe ether solution was dried over MgSO4
6. filtrationfiltered
7. customThe filtrate was taken to dryness in a rotary evaporator