Dichloromethane → N-methyl-N-(2-chlorocyclooctylthio)-N'-(3,4-dichlorophenyl) urea

HRID 268107

반응식

HRID 268107 반응식
[CH2:1]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[S:10][N:11]([CH3:23])[C:12]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[C:17]([Cl:22])[CH:16]=1)=[O:13].C(Cl)[Cl:25]>>[CH3:23][N:11]([S:10][CH:1]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[Cl:25])[C:12]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[C:17]([Cl:22])[CH:16]=1)=[O:13]

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 9266CyclooctaneHCID 21314661N-chlorothio-N-methyl-N'-(3,4-dichlorophenyl) urea

생성물 1

HCID 54070333N-methyl-N-(2-chlorocyclooctylthio)-N'-(3,4-dichlorophenyl) urea

실험 절차

An 11.0-g (0.1 mol) sample of cyclooctane was added dropwise at 0°C. to a solution of 0.1 mol N-chlorothio-N-methyl-N'-(3,4-dichlorophenyl) urea, prepared by a procedure similar to that of Example 3, in methylene dichloride. After the addition was completed, the reaction mixture was washed successively with water, aqueous sodium bicarbonate solution and water, dried over magnesium sulfate and evaporated to give a solid residue. The solid was recrystallized from isopropyl alcohol and washed with hexane to give 15 g of product, m.p. 90°-91°C. Elemental analysis for C16H21Cl3N2OS showed: %S, calc. 8.1, found 8.2; %Cl, calc. 26.9, found 27.4.

후처리

  1. customprepared by a procedure similar to that of Example 3
  2. additionAfter the addition
  3. washthe reaction mixture was washed successively with water, aqueous sodium bicarbonate solution and water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customto give a solid residue
  7. customThe solid was recrystallized from isopropyl alcohol
  8. washwashed with hexane

출처 및 근거

ORD 기록
ord-a2736e8c9947448eb3dc6696adab7f93
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03946062

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