Trichloromethanesulfenyl chloride → HCID 20356007、化合物

HRID 371708

反応式

HRID 371708 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12](=[O:13])[NH:11][NH:10][C:9]2=[O:14])[CH:5]=[CH:6][CH:7]=1.[OH-].[Na+].[Cl:17][C:18]([Cl:22])([Cl:21])[S:19]Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:9](=[O:14])[N:10]([S:19][C:18]([Cl:22])([Cl:21])[Cl:17])[N:11]([S:19][C:18]([Cl:22])([Cl:21])[Cl:17])[C:12]2=[O:13])[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 12855214-(3-Chlorophenyl)-1,2,4-triazolidine-3,5-dione

生成物 1

HCID 20356007HCID 20356007、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

To a solution of 42.2g (0.2 mole) 4-(3-chlorophenyl) urazole in 200 ml water was added a solution of 16g (0.4 mole) sodium hydroxide in 20 ml water. A mixture of 74.4g (0.4 mole) trichloromethylsulfenyl chloride and 3g of an emulsifier solution (as in example 1) in 50 ml water was added dropwise to the above basic solution while keeping the reaction mixture at 0° C. The reactants were mixed so that the reaction mixture was kept at a pH greater than 7. The precipitate that formed was filtered and the filter cake was washed with water. After drying and recrystallizing from cyclohexane there was obtained 70g (69%) 4-(3-chlorophenyl)-1,2-bis-(trichloromethylthio) urazole having a melting point of 153° C.

後処理

  1. additionwas added dropwise to the above basic solution
  2. customat 0° C
  3. additionThe reactants were mixed so that the reaction mixture
  4. customThe precipitate that formed
  5. filtrationwas filtered
  6. washthe filter cake was washed with water
  7. customAfter drying
  8. customrecrystallizing from cyclohexane

出典と根拠

ORDレコード
ord-8e2eb88ab11d40b1a7e10e885feceab1
出典データセット
uspto-grants-1978_05
特許番号
US04087534

関連ノート

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