تفاعل #652354

معادلة التفاعل

tetrahydrofuran

phenoxycarbonylbenzotriazole

bis(trichloromethyl) carbonate

→

phenoxycarbonylbenzotriazole

carbamoyl chloride

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONAfter the solvent was distilled away at reduced pressure, 200 mL of hexane
2. 2
   workup.ADDITIONwere added to the concentrated residue
3. 3
   ترشيحThe crystals were filtered out
4. 4
   أخرىdried

الإجراء التجريبي

A tetrahydrofuran (75 mL) solution of phenoxycarbonylbenzotriazole (19.1 g) was dropped into an ethyl acetate solution (100 mL) of bis(trichloromethyl) carbonate (9.5 g) at 10° C. The resultant solution was stirred at 40° C. for 3 hrs. After the solvent was distilled away at reduced pressure, 200 mL of hexane were added to the concentrated residue, and the material was stirred for 1 hr. The crystals were filtered out and dried to obtain carbamoyl chloride of phenoxycarbonylbenzotriazole (to be abbreviated as PBT-COCl hereinafter) (22.4 g).

المصدر