Dithiodibenzoic acid → 2,2'-Dithiobisbenzol chloride

HRID 1378784

反応式

HRID 1378784 の反応式
C(O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][S:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1C(O)=O.S(Cl)([Cl:23])=O>>[Cl-:23].[CH:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][S:9][C:10]1[CH:11]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

3

反応物 2

HCID 8409Dithiodibenzoic acidHCID 24386Thionyl Chloride

生成物 1

HCID 229131152,2'-Dithiobisbenzol chloride

反応条件

温度
30 °C

実験手順

A mixture of 2,2'-dithiobisbenzoic acid (25 g, 81.6 mmol) in 350 mL of thionyl chloride was heated at reflux for 18 hours. The resulting solution was cooled to about 30° C. and excess thionyl chloride was removed in vacuo. The crude solid was slurried in hexane and the title compound was recovered by filtration to yield 21.2 g. This compound was used without further purification, mp 150°-151° C.;

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. customexcess thionyl chloride was removed in vacuo
  4. filtrationthe title compound was recovered by filtration
  5. customto yield 21.2 g
  6. customThis compound was used without further purification, mp 150°-151° C.

出典と根拠

ORDレコード
ord-50baf349400f4df898a7ae20efc2629e
出典データセット
uspto-grants-1997_09
特許番号
US05668291

関連ノート

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