Succinic anhydride → HCID 14234801, 화합물

HRID 1614030

반응식

HRID 1614030 반응식
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:12])([CH3:11])[CH:3]1[CH3:13].[C:15]1(=[O:21])[O:20][C:18](=[O:19])[CH2:17][CH2:16]1.[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[CH3:11][C:4]1([CH3:12])[C:5]2[C:10](=[CH:9][C:8]([C:15](=[O:21])[CH2:16][CH2:17][C:18]([OH:20])=[O:19])=[CH:7][CH:6]=2)[C:2]([CH3:14])([CH3:1])[CH:3]1[CH3:13]

참가 물질

5

반응물 3

HCID 7922Succinic anhydrideHCID 145491,1,2,3,3-PentamethylindanHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 14234801HCID 14234801, 화합물수율 41.9%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To a solution of 11 g of 1,1,2,3,3-pentamethyl indane (0.058 mole) and 7 g of succinic anhydride (0.07 mole) in 100 cm3 of anhydrous 1,2-dichloroethane, stirred at 0° C, there are added, by small portions, 9.4 g of aluminum chloride in a manner such that the temperature remains lower than 30° C. The reaction mixture is stirred for 3 hours at ambient temperature and then poured into 250 cm3 of ice water. The organic phase is decanted and the aqueous phase is extracted twice with 1,2-dichloroethane. The organic phases are combined, washed with water and dried on magnesium sulfate. The solvent is evaporated under reduced pressure and the resulting product is crystallized in isopropyl ether. 7 g of 4-(1,1,2,3,3-pentamethyl-5-indanyl)-4-oxo butyric acid in the form of white crystals whose melting point is 161° C. are obtained.

후처리

  1. customremains lower than 30° C
  2. customThe organic phase is decanted
  3. extractionthe aqueous phase is extracted twice with 1,2-dichloroethane
  4. washwashed with water
  5. customdried on magnesium sulfate
  6. customThe solvent is evaporated under reduced pressure
  7. customthe resulting product is crystallized in isopropyl ether

출처 및 근거

ORD 기록
ord-2fb428991b964f1482c89dff5f53c9e6
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194663

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