HCID 178418395, 화합물 → HCID 178527778, 화합물

HRID 1460924

반응식

HRID 1460924 반응식
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

참가 물질

5

반응물 2

HCID 178418395HCID 178418395, 화합물HCID 178443003HCID 178443003, 화합물

생성물 1

HCID 178527778HCID 178527778, 화합물수율 397.2%

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7539f7318a214fb0a64287daa8aff749
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05073279

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