Hydrogen Peroxide → 3,4-Epoxy-1-(beta,beta,beta-trichloroethoxycarbonyl)-pyrrolidine

12 ml of 90% strength hydrogen peroxide (0.48 mol) are dissolved in 40 ml of methylene chloride and the solution is treated at 0° with 63.5 ml (0.45 mol) of trifluoroacetic anhydride. After stirring for 15 minutes at 0°, the solution is added dropwise to a suspension, which is kept at 0°, of 196 g of anhydrous disodium hydrogen phosphate in 800 ml of methylene chloride, in which 41.8 g (0.17 mol) of N-(β,β,β-trichloroethoxycarbonyl)-3-pyrroline has been dissolved. Subsequently, the reaction mixture is stirred for 2 hours at room temperature and then stirred into 900 ml of water and the resulting mixture is stirred for a further one hour. The organic phase is separated off and the aqueous phase is extracted by shaking with 3 times 200 ml of methylene chloride; the combined organic phases are washed successively with aqueous sodium chloride solution, aqueous iron-II sulphate solution and then with water, dried over sodium sulphate and evaporated under a water pump vacuum, whereupon 3,4-epoxy-1-(β,β,β-trichloroethoxycarbonyl)-pyrrolidine is obtained in the form of white crystals with a melting point of 52°-55°.

1. additionthe solution is added dropwise to a suspension, which
2. dissolutionhas been dissolved
3. stirringSubsequently, the reaction mixture is stirred for 2 hours at room temperature
4. stirringthe resulting mixture is stirred for a further one hour
5. customThe organic phase is separated off
6. extractionthe aqueous phase is extracted
7. stirringby shaking with 3 times 200 ml of methylene chloride
8. washthe combined organic phases are washed successively with aqueous sodium chloride solution, aqueous iron-II sulphate solution
9. dry with materialwith water, dried over sodium sulphate
10. customevaporated under a water pump vacuum

ORDレコード

ord-85b997f624914520a9bfedb084b3a539

出典データセット

uspto-grants-1981_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04246269