Potassium Iodide → N-[2-(Phenylthio)ethyl]-2-propanamine hydrochloride

HRID 4206

반응식

HRID 4206 반응식
[C:1]1([S:7][CH2:8][CH2:9][Cl:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[I-].[K+].[CH:13]([NH2:16])([CH3:15])[CH3:14]>>[ClH:10].[C:1]1([S:7][CH2:8][CH2:9][NH:16][CH:13]([CH3:15])[CH3:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 3

HCID 4875Potassium IodideHCID 6363IsopropylamineHCID 21702((2-Chloroethyl)thio)benzene

생성물 1

HCID 13655077N-[2-(Phenylthio)ethyl]-2-propanamine hydrochloride수율 76.9%

실험 절차

A solution of 25 g (0.145 mole) of 2-chloroethyl phenyl sulfide and 1 g (0.006 mole) of potassium iodide in 500 ml of isopropylamine was heated in a bomb at 120° C. for 24 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was extracted with dilute sulfuric acid. The acidic extract was made basic with 50% sodium hydroxide, and the basic solution was extracted with methylene chloride. The methylene chloride solution was dried over magnesium sulfate and the solvent was removed in vacuo to give an oil. This was converted to the hydrochloride salt, and the salt was recrystallized from methanol-ether to give 25.77 g (76.9%) of white crystalline solid, m.p. 124.5°-125.5° C.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
  3. extractionThe methylene chloride solution was extracted with dilute sulfuric acid
  4. extractionThe acidic extract
  5. extractionthe basic solution was extracted with methylene chloride
  6. dry with materialThe methylene chloride solution was dried over magnesium sulfate
  7. customthe solvent was removed in vacuo
  8. customto give an oil
  9. customthe salt was recrystallized from methanol-ether

출처 및 근거

ORD 기록
ord-7339c7a207114a058f08a02bd2cd46d8
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04724235

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