HCID 178418395、化合物 → HCID 178527778、化合物

HRID 1589712

反応式

HRID 1589712 の反応式
CCCCCCCCCCCCCCCCC=C.[S:19][Cl:20].[SH:21][C:22]1[S:23][C:24]2[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=2[N:26]=1>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C1(C)C=CC=CC=1>[S:19][Cl:20].[SH:21][C:22]1[S:23][C:24]2[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=2[N:26]=1

参加物

5

反応物 2

HCID 178418395HCID 178418395、化合物HCID 178443003HCID 178443003、化合物

生成物 1

HCID 178527778HCID 178527778、化合物収率 397.2%

試薬・触媒・溶媒 2

HCID 21218Trioctylmethylammonium chloride触媒HCID 1140Toluene溶媒

実験手順

278.4 gm of the product of Example 1 (0.4 mol.), 133.8 gm of 2-mercaptobenzothiazole (0.8 mol.), 8 gm of Aliquat 336 (phase transfer catalyst obtained from Aldrich Chemical Company: tricaprylylmethyl ammonium chloride), 200 ml caustic solution (32 gm sodium hydroxide dissolved in 200 ml water), and 400 ml toluene were mixed in a 2-liter reactor. The reactants were stirred under reflux for six hours, and then cooled to ambient temperature. The aqueous phase was separated, and the organic phase was twice washed with 400 ml of water. Thereafter, toluene was removed by vacuum distillation leaving a dark fluid as the desired product (373 gm). It was further purified by hot filtration through Super-Cel.

後処理

  1. temperatureunder reflux for six hours
  2. customThe aqueous phase was separated
  3. washthe organic phase was twice washed with 400 ml of water
  4. customThereafter, toluene was removed by vacuum distillation

出典と根拠

ORDレコード
ord-6fe259680bc6441d8d271f5006828699
出典データセット
uspto-grants-1993_04
特許番号
US05199960

関連ノート

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