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Thionyl Chloride → HCID 53773575, 화합물

HRID 6323
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반응식

HRID 6323 반응식
[CH2:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16](O)=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]=[CH2:10].S(Cl)([Cl:23])=O>C1(C)C=CC=CC=1>[CH:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([Cl:23])=[O:17])=[CH:14][CH:13]=1)=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
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참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 148765254-(9-Decen-1-yloxy)benzoic acid

생성물 1

HCID 53773575HCID 53773575, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To 2.8 g of p-(9-decenyloxy)benzoic acid prepared in the same manner as in 9.(2) in Example 9 added was toluene, and the resulting mixture was cooled in an ice bath. 5.0 g of thionyl chloride was then added dropwise to the toluene solution. Reaction was then carried out for 7 hours at 80° C. After conclusion of the reaction, the reaction solution was concentrated under reduced pressure, to obtain crude p-decenyloxybenzoyl chloride. 1.6 g of the hydroxy compound obtained in 17.(1) and 3.3 g of pyridine were dissolved in toluene, and the resulting toluene solution was cooled in an ice bath. A toluene solution containing the above crude p-decenyloxybenzoyl chloride was added dropwise into the toluene solution. Subsequently, reaction was carried out for 5 hours at 50° C. After conclusion of the reaction, the reaction solution was washed with water and dried over magnesium sulfate, and the solvent was distilled out under reduced pressure. The residue was purified by column chromatography, to obtain 2.0 g of the objective alkene compound. (Yield: 69%)

후처리

  1. additionadded
  2. temperaturethe resulting mixture was cooled in an ice bath
  3. customReaction
  4. customAfter conclusion of the reaction
  5. concentrationthe reaction solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-91bea4c5979044409b42d000b2acefe8
출처 데이터셋
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05248446

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