Sodium Sulfide → Bis(2,6-dichlorobenzyl) sulfide

HRID 6286

反応式

HRID 6286 の反応式
[S-2:1].[Na+].[Na+].[Cl:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:6]=1[CH2:7]Cl>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[Cl:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:6]=1[CH2:7][S:1][CH2:7][C:6]1[C:5]([Cl:4])=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:13]

参加物

5

反応物 2

HCID 14804Sodium SulfideHCID 748322,6-Dichlorobenzyl chloride

生成物 1

HCID 20404720Bis(2,6-dichlorobenzyl) sulfide収率 80.4%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 962Water溶媒

実験手順

A mixture of 98.8 g (0.411 mol) of sodium sulfide, 5.0 g of tetrabutylammonium hydrogen sulfate and 110 ml of water are stirred in a reaction vessel equipped with a stirrer, thermometer and heatable dropping funnel, until a solution is obtained. 107.2 g of melted 2,6-dichlorobenzyl chloride are added with vigorous stirring over a period of 25 minutes at such a rate that the inside temperature does not exceed 55° C. The reaction mixture is worked up as in Example 9a) to give 77.6 g (80% of theory) of bis(2,6-dichlorobenzyl) sulfide in the form of white crystals of melting point 128°-130° C.

後処理

  1. customequipped with a stirrer
  2. customuntil a solution is obtained
  3. stirringwith vigorous stirring over a period of 25 minutes at such a rate that the inside temperature
  4. customdoes not exceed 55° C

出典と根拠

ORDレコード
ord-36a943ae44634d7499c53401c1d522ef
出典データセット
uspto-grants-1993_09
特許番号
US05247113

関連ノート

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