4-Vinylbenzoic acid → 4-Vinylbenzoyl chloride

HRID 404305

반응식

HRID 404305 반응식
[CH:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](O)=[O:8])=[CH:5][CH:4]=1)=[CH2:2].S(Cl)([Cl:14])=O>CN(C)C=O.C1(C)C=CC=CC=1>[CH:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([Cl:14])=[O:8])=[CH:5][CH:4]=1)=[CH2:2]

참가 물질

5

반응물 2

HCID 140984-Vinylbenzoic acidHCID 24386Thionyl Chloride

생성물 1

HCID 110520284-Vinylbenzoyl chloride수율 70%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

While 16.6 g of p-vinylbenzoic acid (manufactured by Wako Pure Chemical Industries, Ltd.), 80 ml of toluene, two drops of N,N-dimethylformamide were stirred at room temperature, 9.7 ml of thionyl chloride (manufactured by Wako Pure Chemical Industries, Ltd.) was added thereto, which was heated and stirred at 60° C. for 2 hours. The inside of the reaction system was cooled to 40° C., toluene and an excessive amount of thionyl chloride were removed under reduced pressure, and p-vinyl benzoic acid chloride was obtained. While 22.5 g of 2-aminoanthraquinone (manufactured by Tokyo Chemical Industry Co., Ltd.) and 110 ml of pyridine were stirred on ice, p-vinyl benzoic acid chloride was slowly added dropwise thereto. After stirring the mixture on ice for 30 minutes, the temperature was increased to 60° C. and the mixture was heat while stirring for 3 hours. Thereafter, the mixture was cooled to room temperature and water was added thereto. The resulting coarse crystals were filtrated and washed with water and methanol, and then 500 ml of methanol was added to the collected coarse crystals, and then heated while stirring at 60° C. Thereafter, the resultant crystals were separated by filtration, washed with methanol and dried. Thus, 20.1 g of M-19 was obtained (yield: 70%).

후처리

  1. temperaturewhich was heated
  2. temperatureThe inside of the reaction system was cooled to 40° C.
  3. customtoluene and an excessive amount of thionyl chloride were removed under reduced pressure

출처 및 근거

ORD 기록
ord-11504d18f3af4c2d931f0c94da90fd80
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748529B2

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