Chloroform → 7-cyano-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

HRID 1607556ノート

反応式

HRID 1607556 の反応式
[CH2:1]([S:7][C:8]1[S:18][C:11]2=[N:12][C:13](I)=[CH:14][C:15](=[O:16])[N:10]2[N:9]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[Cu](C#N)[C:20]#[N:21].[C-]#N.[Na+].C(Cl)(Cl)Cl>CN(C)C=O.O>[C:20]([C:13]1[N:12]=[C:11]2[S:18][C:8]([S:7][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])=[N:9][N:10]2[C:15](=[O:16])[CH:14]=1)#[N:21]

参加物

7

反応物 4

HCID 6212ChloroformHCID 8929Sodium CyanideHCID 156107912-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-oneHCID 178418260HCID 178418260、化合物

生成物 1

HCID 146950717-cyano-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one収率 51.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

In 100 ml of dimethylformamide, 6 g of 2-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was dissolved. To this solution, 1.77 g of copper cyanide and 0.97 g of sodium cyanide were added and the solution was stirred at 100° C. for 1 hour. After the reaction mixture was cooled to room temperature, it was wxtracted with chloroform and water. The organic layer was washed with water and dried over anhydrous sodium sulfate. Florisil® was added to the organic layer and it was shaken. The solvent was distilled off, and 2.3 g of 7-cyano-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained.

後処理

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. additionFlorisil® was added to the organic layer and it
  5. stirringwas shaken
  6. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-98bdf601a9624a9d8a151cc53896db8a
出典データセット
uspto-grants-1989_09
特許番号
US04866064

反応ノート

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