반응 #63165

반응 방정식

hydrogen chloride

phosgene

4-butyrolactone

phosgene

hydrogen chloride

phosgene

→

4-chlorobutyryl chloride

butyrolactone

반응 조건

후처리

1. 1
   기타set at -20° C. and -70° C.
2. 2
   기타are passed in over 5.5 hours
3. 3
   workup.DISTILLATIONWorking up by distillation

실험 절차

430 parts of 4-butyrolactone and 47 parts of trimethylbenzylammonium chloride are initially taken in a 1 l stirred reactor which is equipped with a thermometer, inlet tubes for phosgene and hydrogen chloride and 2 low-temperature coolers set at -20° C. and -70° C. respectively. The mixture is heated to 130° C. 560 parts of phosgene and 120 parts of hydrogen chloride are passed in over 5.5 hours. Thereafter, nitrogen is passed in until the reaction mixture no longer contains any phosgene. Working up by distillation gives 620 g of 4-chlorobutyryl chloride and 30.5 g of butyrolactone. The distillation residue of 75 g, which consists of the catalyst and chlorobutyroyloxybutyryl chloride, can be reused for further batches. The yield of 4-chlorobutyryl chloride is 88 mol %, based on butyrolactone used.

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