Sodium Hydroxide → HCID 178484362, 화합물

HRID 1073814노트

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HRID 1073814 반응식
[SH:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.[OH-].[Na+].[CH3:10][N:11]([CH3:16])[C:12](=[NH:15])[CH2:13]Cl>C(O)C>[CH3:10][N:11]([CH3:16])[C:12]([CH2:13][S:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1)=[NH:15]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 426331Ethanimidamide, 2-chloro-N,N-dimethyl-HCID 178418558HCID 178418558, 화합물

생성물 1

HCID 178484362HCID 178484362, 화합물수율 53.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 30 ml of ethanol was suspended 2.25 g of 2,5-dimercapto-1,3,4-thiadiazole, and 30 ml of 1N-sodium hydroxide solution was added to the suspension. The mixture was stirred at room temperature for 30 minutes. To the mixture was added 2.36 g of N,N-dimethylchloroacetamidine. The mixture was stirred at room temperature for an hour and concentrated under reduced pressure. The precipitating crystals were collected by filtration and washed with cold water and then a (1:1) mixture of methanol and ethyl ether to obtain 1.87 g of 2-(N,N-dimethylamidinomethylthio)-5-mercapto-1,3,4-thiadiazole as colorless crystals (mp 95°-97° C.).

후처리

  1. additionwas added to the suspension
  2. stirringThe mixture was stirred at room temperature for an hour
  3. concentrationconcentrated under reduced pressure
  4. filtrationThe precipitating crystals were collected by filtration
  5. washwashed with cold water
  6. additiona (1:1) mixture of methanol and ethyl ether

출처 및 근거

ORD 기록
ord-a9b698dfb69a4a9794909e1eeef5c81b
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971963

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