反応 #355289

反応方程式

methylene dichloride

cyclooctane

N-chlorothio-N-methyl-N'-(3,4-dichlorophenyl) urea

→

product

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

反応条件

後処理

1. 1
   その他prepared by a procedure similar to that of Example 3
2. 2
   workup.ADDITIONAfter the addition
3. 3
   洗浄the reaction mixture was washed successively with water, aqueous sodium bicarbonate solution and water
4. 4
   乾燥dried over magnesium sulfate
5. 5
   その他evaporated
6. 6
   その他to give a solid residue
7. 7
   その他The solid was recrystallized from isopropyl alcohol
8. 8
   洗浄washed with hexane

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.

出典