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

HRID 1105879

반응식

HRID 1105879 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-7418178551d446d4aeac9a32f44bb6f8
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04310590

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