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Ethyl Acetate → Benzyl4-[[(5,5-dimethyl-5,6,7,8-tetrahydro-8-oxo-naphthalen-2-yl)carbonyl]oxy]-benzoate

HRID 992141
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HRID 992141 반응식
[CH3:1][C:2]1([CH3:16])[CH2:11][CH2:10][C:9](=[O:12])[C:8]2[CH:7]=[C:6]([C:13]([OH:15])=[O:14])[CH:5]=[CH:4][C:3]1=2.CN([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22]N=1)C.[C:26]([O:29][CH2:30][CH3:31])(=[O:28])[CH3:27]>CN(C)C=O>[CH2:30]([O:29][C:26](=[O:28])[C:27]1[CH:10]=[CH:11][C:2]([O:14][C:13]([C:6]2[CH:5]=[CH:4][C:3]3[C:2]([CH3:16])([CH3:1])[CH2:11][CH2:10][C:9](=[O:12])[C:8]=3[CH:7]=2)=[O:15])=[CH:3][CH:8]=1)[C:31]1[CH:20]=[CH:25][CH:24]=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 218852-DimethylaminopyridineHCID 154628445,5-Dimethyl-8-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylic acid2회

생성물 1

HCID 22641986Benzyl4-[[(5,5-dimethyl-5,6,7,8-tetrahydro-8-oxo-naphthalen-2-yl)carbonyl]oxy]-benzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5,5-dimethyl-5,6,7,8-tetrahydro-8-oxo-naphthalen-2-carboxylic acid (Compound E3, 386 mg, 1.77 mmol) in dimethylformamide (4 mL) was added 1-(3-dimethylaminopropyl)-3-ethylcarboimide hydrochlorde (440 mg, 2.3 mmol) followed by dimethylamino pyridine (DMAP) (280 mg, 2.3 mmol). The mixture was stirred for 10 minutes, and benzyl 4-hydroxy benzoate (426 mg, 1.9 mmol) was added and stirred at ambient temperature for 16 hours. The mixture was diluted with ethyl acetate (100 mL) and washed with water (10 mL), brine (10 mL), dried and solvent distilled off. The title compound was obtained as a pale yellow solid after chromatographic purification.

후처리

  1. stirringstirred at ambient temperature for 16 hours
  2. washwashed with water (10 mL), brine (10 mL)
  3. customdried
  4. distillationsolvent distilled off

출처 및 근거

ORD 기록
ord-9ca5f611a7d7495cb9b848388d560e17
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06465663B2

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