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

HRID 268107

反応式

HRID 268107 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a2736e8c9947448eb3dc6696adab7f93
出典データセット
uspto-grants-1976_03
特許番号
US03946062

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