1-(5-Chloro-2-(methylthio)pyrimidine-6-carbonyl)-4-(4-fluorophenyl)thiosemicarbazide → 5-(5-Chloro-2-(methylthio)pyrimidin-4-yl)-N-(4-fluorophenyl)-1,3,4-thiadiazol-2-amine

HRID 507642ノート

反応式

HRID 507642 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([S:22][CH3:23])=[N:6][C:7]=1[C:8]([NH:10][NH:11][C:12]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=1)=[S:13])=O>S(=O)(=O)(O)O.O>[Cl:1][C:2]1[C:7]([C:8]2[S:13][C:12]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)=[N:11][N:10]=2)=[N:6][C:5]([S:22][CH3:23])=[N:4][CH:3]=1

参加物

4

反応物 1

HCID 602045491-(5-Chloro-2-(methylthio)pyrimidine-6-carbonyl)-4-(4-fluorophenyl)thiosemicarbazide

生成物 1

HCID 602045505-(5-Chloro-2-(methylthio)pyrimidin-4-yl)-N-(4-fluorophenyl)-1,3,4-thiadiazol-2-amine収率 71%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

1-(5-Chloro-2-(methylthio)pyrimidine-6-carbonyl)-4-(4-fluorophenyl)thiosemicarbazide (1.08 g, 2.9 mmol) was diluted in 60 mL sulfuric acid. This solution was stirred at room temperature for 5 min before cooling in an ice bath. The reaction mixture was carefully diluted with excess H2O forming the product as a bright orange ppt. The product was collected by filtration and dried in a vacuum oven overnight to give 0.721 g (71% yield) of product as a bright orange solid. MS (M+H)+ 354.

後処理

  1. temperaturebefore cooling in an ice bath
  2. filtrationThe product was collected by filtration
  3. customdried in a vacuum oven overnight

出典と根拠

ORDレコード
ord-925c5b881f6049c0b581d989b8de5e2e
出典データセット
uspto-grants-2010_08
特許番号
US07786132B2

反応ノート

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