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Sodium Hydroxide → 4-(Dimethylamino)butanethiol hydrochloride

HRID 266873
ノート
印刷プレビュー

反応式

HRID 266873 の反応式
[OH-].[Na+].[ClH:3].Cl.[CH3:5][N:6]([CH3:15])[CH2:7][CH2:8][CH2:9][CH2:10][S:11]C(=N)N>O>[ClH:3].[CH3:5][N:6]([CH3:15])[CH2:7][CH2:8][CH2:9][CH2:10][SH:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 11957708SKF 91488 dihydrochloride

生成物 1

HCID 190315554-(Dimethylamino)butanethiol hydrochloride収率 60.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
95 °C

実験手順

A solution of sodium hydroxide (16.4 g) in water (16.5 ml) was added dropwise under nitrogen at 0° C. to a stirred solution of S-[4-(dimethylamino)butyl]-isothiourea dihydrochloride (51 g) in water (60 ml), then the mixture was heated at 95° C. for 2 hours and allowed to cool to ambient temperature. Water (100 ml) was added, and the product was extracted into ether (50 ml), dichloromethane (3×50 ml), and ether (2×50 ml). The combined organic solutions were dried over magnesium sulphate, then the solvents were removed in vacuo. The residue was dissolved in ether and the solution was saturated with hydrogen chloride. The resulting solid was collected by filtration and dried in vacuo at ambient temperature to give 4-(dimethylamino)butanethiol hydrochloride as a white solid (21 g) which was used without further purification.

後処理

  1. temperatureto cool to ambient temperature
  2. extractionthe product was extracted into ether (50 ml), dichloromethane (3×50 ml), and ether (2×50 ml)
  3. dry with materialThe combined organic solutions were dried over magnesium sulphate
  4. customthe solvents were removed in vacuo
  5. dissolutionThe residue was dissolved in ether
  6. filtrationThe resulting solid was collected by filtration
  7. customdried in vacuo at ambient temperature

出典と根拠

ORDレコード
ord-1f64c6af0f0b4255a5feb84bf4e8c6c9
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05652271

反応ノート

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