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

HRID 6286
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인쇄 미리보기

반응식

HRID 6286 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14804Sodium SulfideHCID 748322,6-Dichlorobenzyl chloride

생성물 1

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

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-36a943ae44634d7499c53401c1d522ef
출처 데이터셋
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05247113

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