HCID 54250551, 화합물 → N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamine

HRID 4195노트

반응식

HRID 4195 반응식
C1(OC(=O)[N:9]([CH2:13][CH2:14][S:15]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=2)(=[O:17])=[O:16])[CH:10]([CH3:12])[CH3:11])C=CC=CC=1>Br>[Cl:25][C:20]1[CH:19]=[C:18]([S:15]([CH2:14][CH2:13][NH:9][CH:10]([CH3:12])[CH3:11])(=[O:16])=[O:17])[CH:23]=[CH:22][C:21]=1[Cl:24]

참가 물질

3

반응물 1

HCID 54250551HCID 54250551, 화합물

생성물 1

HCID 14050280N-[2-[(3,4-Dichlorophenyl)sulfonyl]ethyl]-2-propanamine수율 32.4%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

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.

후처리

  1. temperatureat reflux for 12 hr
  2. extractionextracted with chloroform
  3. extractionThe chloroform layer was extracted with 1N sulfuric acid
  4. extractionThe sulfuric acid layer was extracted with chloroform
  5. customevaporated to an oil
  6. customA portion of the oil was reacted with ethereal hydrogen chloride

출처 및 근거

ORD 기록
ord-ac7bb16995024c46a7800aead047370a
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04724235

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