Sodium Hydroxide → HCID 178484362、化合物

HRID 1073814ノート

反応式

HRID 1073814 の反応式
[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]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 426331Ethanimidamide, 2-chloro-N,N-dimethyl-HCID 178418558HCID 178418558、化合物

生成物 1

HCID 178484362HCID 178484362、化合物収率 53.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-a9b698dfb69a4a9794909e1eeef5c81b
出典データセット
uspto-grants-1990_11
特許番号
US04971963

反応ノート

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