반응 #4291

ord-ac7bb16995024c46a7800aead047370a

반응 방정식

CC(C)N(CCS(=O)(=O)c1ccc(Cl)c(Cl)c1)C(=O)Oc1ccccc1
N-[2-[(3,4-dichlorophenyl)sulfonyl]ethyl]-N-(1-methylethyl)carbamic acid phenyl ester
CC(C)NCCS(=O)(=O)c1ccc(Cl)c(Cl)c1
white crystalline product
수율 32.4%
CC(C)NCCS(=O)(=O)c1ccc(Cl)c(Cl)c1
N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamine
수율 32.4%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 12 hr
  2. 2
    추출extracted with chloroform
  3. 3
    추출The chloroform layer was extracted with 1N sulfuric acid
  4. 4
    추출The sulfuric acid layer was extracted with chloroform
  5. 5
    기타evaporated to an oil
  6. 6
    기타A portion of the oil was reacted with ethereal hydrogen chloride

실험 절차

A solution of 44.27 g (0.107 mole of N-[2-[(3,4-dichlorophenyl)sulfonyl]ethyl]-N-(1-methylethyl)carbamic acid phenyl ester in 300 ml of 48% HBr was heated at reflux for 12 hr. The reaction mixture was cooled to room temperature, made alkaline with 50% sodium hydroxide-ice and extracted with chloroform. The chloroform layer was extracted with 1N sulfuric acid. The sulfuric acid layer was extracted with chloroform and the chloroform layers combined and evaporated to an oil, the free base of the title compound. A portion of the oil was reacted with ethereal hydrogen chloride to give an overall yield of 32.4% white crystalline product, m.p. 219°-221° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04724235uspto-grants-1988_02