反应详情

35.7 g of isopropyl 2-chloroacetate is added to a suspension of 33.5 g of 4-phenylthiosemicarbazide in 150 ml of tetrahydrofuran. After the mixture has been stirred for 30 minutes it is boiled for a further 30 minutes and then allowed to cool. The precipitated solid is isolated by suction filtering, washed with acetone and the residue is heated in a water/acetone mixture (1:1). After the separated sulfur has been poured off, the whole is allowed to cool and is neutralized with aqueous NaHCO3, solution and the precipitated solid is isolated; m.p. 138°-139° C. (from toluene).

1. waitis boiled for a further 30 minutes
2. temperatureto cool
3. customThe precipitated solid is isolated by suction
4. filtrationfiltering
5. washwashed with acetone
6. temperaturethe residue is heated in a water/acetone mixture (1:1)
7. additionAfter the separated sulfur has been poured off
8. temperatureto cool
9. customthe precipitated solid is isolated