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

HRID 745162ノート

反応式

HRID 745162 の反応式
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]

参加物

3

反応物 1

HCID 54250551HCID 54250551、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

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 crystaline product, m.p. 219°-221° C.

後処理

  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

出典と根拠

ORDレコード
ord-5665680ad6fd4ce0aa03580362069ac6
出典データセット
uspto-grants-1986_07
特許番号
US04597902

反応ノート

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