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

HRID 4206

反応式

HRID 4206 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7339c7a207114a058f08a02bd2cd46d8
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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