Hydrochloric Acid → 4,4-Dimethyl-2-(4'hydroxymethylbiphenyl-2-yl)oxazoline

HRID 742787

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HRID 742787 반응식
[CH3:1][C:2]1([CH3:24])[CH2:6][O:5][C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:18]=[CH:17][C:16]([CH2:19][O:20]COC)=[CH:15][CH:14]=2)=[N:3]1.Cl.C(=O)([O-])O.[Na+].C(=O)([O-])[O-]>CO>[CH3:1][C:2]1([CH3:24])[CH2:6][O:5][C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:14]=[CH:15][C:16]([CH2:19][OH:20])=[CH:17][CH:18]=2)=[N:3]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 19660Carbonate IonHCID 516892Sodium BicarbonateHCID 118343424,4-Dimethyl-2-(4'-methoxymethoxymethylbiphenyl-2-yl)oxazoline

생성물 1

HCID 110658764,4-Dimethyl-2-(4'hydroxymethylbiphenyl-2-yl)oxazoline수율 97.1%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

2.62 g (8.05 mmol) of 4,4-dimethyl-2-(4'-methoxymethoxymethylbiphenyl-2-yl)oxazoline was dissolved in methanol (20 ml). 6N hydrochloric acid (10 ml) was added thereto, followed by stirring at 40° C. for 2 hours. The reaction liquid was poured into a saturated aqueous solution of sodium hydrogen-carbonate, carbonate, followed by the extraction with chloroform. After washing with water and drying, vacuum concentration was conducted. The residue was purified by silica gel column chromatography (a n-hexane/ethyl acetate system) to give 2.20 g of the title compound as a crystal (yield 97%).

후처리

  1. customThe reaction liquid
  2. extractionfollowed by the extraction with chloroform
  3. washAfter washing with water
  4. customdrying
  5. concentrationvacuum concentration
  6. customThe residue was purified by silica gel column chromatography (a n-hexane/ethyl acetate system)

출처 및 근거

ORD 기록
ord-f35ec2ce088b44e3b9b3aa4c6b518e05
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554757

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