Water → N-[2-[(4-Chlorophenyl)thio]ethyl]-1-methylethanamine hydrochloride

HRID 4187

反応式

HRID 4187 の反応式
[Cl:1]CCC1C=C(Cl)C=[CH:6][C:5]=1[S:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1CCCl.O.C(Cl)(Cl)Cl.[CH:27]([NH2:30])([CH3:29])[CH3:28]>>[ClH:1].[Cl:18][C:15]1[CH:14]=[CH:13][C:12]([S:11][CH2:5][CH2:6][NH:30][CH:27]([CH3:29])[CH3:28])=[CH:17][CH:16]=1

参加物

5

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 6363IsopropylamineHCID 54258412Chloroethyl-p-chlorophenyl sulfide

生成物 1

HCID 13655027N-[2-[(4-Chlorophenyl)thio]ethyl]-1-methylethanamine hydrochloride

実験手順

A solution of 24.0 g (0.116 mole) chloroethyl-p-chlorophenyl sulfide in 100 ml of isopropylamine was agitated overnight in a stainless steel bomb at 80° C. The reaction mixture was then stripped to dryness and the residue partitioned between water and chloroform. The chloroform layer was extracted with 1N sulfuric acid. Three layers were obtained: a water phase (lower), a chloroform phase (upper) and an intermediate phase. The aqueous and intermediate phases were combined, made alkaline and extracted with chloroform. Evaporation yielded an oil, the free base of the title compound. A portion of the oil was reacted with ethereal hydrogen chloride and the resulting hydrochloride salt was recrystallized from methanol-diethyl ether to give 2.23 g (22.6%) of white crystalline product, m.p. 126°-128° C.

後処理

  1. customthe residue partitioned between water and chloroform
  2. extractionThe chloroform layer was extracted with 1N sulfuric acid
  3. customThree layers were obtained
  4. extractionextracted with chloroform
  5. customEvaporation
  6. customyielded an oil

出典と根拠

ORDレコード
ord-ad0a48963d2543e0863f057522180da5
出典データセット
uspto-grants-1988_02
特許番号
US04724235

関連ノート

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