Trichloromethanesulfenyl chloride → HCID 20356007, 화합물

HRID 371708

반응식

HRID 371708 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 20356007HCID 20356007, 화합물

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8e2eb88ab11d40b1a7e10e885feceab1
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04087534

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