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Hydrochloric Acid → HCID 86733122, 화합물

HRID 267595
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HRID 267595 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6](C)[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH3:12])[CH3:2].[C:14]1(=[O:20])[O:19][C:17](=[O:18])[CH2:16][CH2:15]1.[Cl-].[Al+3].[Cl-].[Cl-].Cl.[CH2:26](Cl)Cl>C(Cl)(Cl)(Cl)Cl>[CH3:26][CH2:12][CH2:11][O:10][C:9]1[C:4]([O:3][CH2:1][CH3:2])=[CH:5][CH:6]=[C:7]([CH:8]=1)[C:17]([CH2:16][CH2:15][C:14]([OH:19])=[O:20])=[O:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 7922Succinic anhydrideHCID 757883,4-DiethoxytolueneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 86733122HCID 86733122, 화합물

시약·촉매·용매 1

HCID 5943
Carbon Tetrachloride
용매

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온도
25 °C

실험 절차

To the mixture of 9.0 parts by weight of 3,4-diethoxytoluene, 6.0 parts by weight of succinic anhydride and 100 parts by volume of carbon tetrachloride is added 27 parts by weight of anhydrous aluminum chloride. The mixture is stirred for 1 hour at 25°C and mildly refluxed for 2 hours. After cooling, 70 parts by weight of ice and 70 parts by volume of concentrated hydrochloric acid are added to the mixture and thereto is further added methylenedichloride and the whole mixture is shaken. The organic solvent layer is separated and extracted with a 2N-aqueous solution of sodium carbonate. The aqueous solution is adjusted with diluted hydrochloric acid to pH 2.5, whereby 3-(2'-methyl-4',5'-diethoxybenzoyl)-propionic acid is obtained as crystals. Recrystallization of the crystals gives 10.0 parts by weight of colorless plates melting at 116°-117°C.

후처리

  1. temperaturemildly refluxed for 2 hours
  2. temperatureAfter cooling
  3. stirringthe whole mixture is shaken
  4. customThe organic solvent layer is separated
  5. extractionextracted with a 2N-aqueous solution of sodium carbonate

출처 및 근거

ORD 기록
ord-47f2c6ff12d94ff98c12031d007d4c4e
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03943169

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