Trichloromethanesulfenyl chloride → 4-(4-Chlorophenyl)-1, 2-bis(trichloromethylthio)urazole

HRID 371709

반응식

HRID 371709 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[NH:11][NH:10][C:9]2=[O:14])=[CH:4][CH:3]=1.[OH-].[Na+].[Cl:17][C:18]([Cl:22])([Cl:21])[S:19]Cl>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([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:6][CH:7]=1

참가 물질

5

반응물 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 53055984-(4-Chlorophenyl)-1,2,4-triazolidine-3,5-dione

생성물 1

HCID 203559844-(4-Chlorophenyl)-1, 2-bis(trichloromethylthio)urazole

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

To a solution of 42.2g (0.2 mole) 4-(4-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 was formed was collected on a filter and the filter cake was washed with water. After drying, triturating with ethyl ether, and recrystallizing from benzene-cyclohexane (1:1, by volume) there was obtained 42g (64%) of 4-(4-chlorophenyl)-1, 2-bis(trichloromethylthio)urazole having a melting point of 169° 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 was formed
  5. customwas collected on
  6. filtrationa filter
  7. washthe filter cake was washed with water
  8. customAfter drying
  9. customtriturating with ethyl ether
  10. customrecrystallizing from benzene-cyclohexane (1:1, by volume) there

출처 및 근거

ORD 기록
ord-6c4eac9d8d0b46a889b1b73f58176d25
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04087534

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