Sodium Iodide → 2-Benzyl-5-(N,N-dimethylthiocarbamoyl)thio-4-isothiazolin-3-one

HRID 1105879

反応式

HRID 1105879 の反応式
[CH2:1]([N:8]1[C:12](=[O:13])[CH:11]=[C:10](Cl)[S:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.[Na+].[CH3:18][N:19]([CH3:23])[C:20](=[S:22])[S-:21].[I-].[Na+]>C(O)C>[CH2:1]([N:8]1[C:12](=[O:13])[CH:11]=[C:10]([S:22][C:20](=[S:21])[N:19]([CH3:23])[CH3:18])[S:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 43451522-benzyl-5-chloroisothiazol-3(2H)-oneHCID 23693613Sodium dimethyldithiocarbamate dihydrate

生成物 1

HCID 128527272-Benzyl-5-(N,N-dimethylthiocarbamoyl)thio-4-isothiazolin-3-one収率 60%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of 6.76 g. (0.03 mole) of 2-benzyl-5-chloro-4-isothiazolin-3-one in 25 ml of ethanol was added a solution of 5.37 g. (0.03 mole) of N,N-dimethyldithiocarbamic acid sodium salt dihydrate in 30 ml of ethanol followed by 0.1 g. of sodium iodide. A yellow solid separated spontaneously. The mixture was stirred at room temperature for 3 hours, then cooled and filtered. The solid was triturated with 50 ml of water and recrystallized from 250 ml of boiling EtOH to give 5.6 g. (60% yield) of the named product, mp 184°-186°.

後処理

  1. customA yellow solid separated spontaneously
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe solid was triturated with 50 ml of water
  5. customrecrystallized from 250 ml of boiling EtOH
  6. customto give 5.6 g

出典と根拠

ORDレコード
ord-7418178551d446d4aeac9a32f44bb6f8
出典データセット
uspto-grants-1982_01
特許番号
US04310590

関連ノート

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