Ethyl chloroacetate → HCID 86729430, 화합물

HRID 629519노트

반응식

HRID 629519 반응식
[C:1]12([C:11]3[CH:16]=[CH:15][C:14]([OH:17])=[C:13]([CH3:18])[CH:12]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28]>CN(C)C=O.C(OCC)(=O)C>[C:1]12([C:11]3[CH:16]=[CH:15][C:14]([O:17][CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:13]([CH3:18])[CH:12]=3)[CH2:8][CH:7]3[CH2:9][CH:3]([CH2:4][CH:5]([CH2:6]3)[CH2:10]1)[CH2:2]2

참가 물질

6

반응물 3

HCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 27950214-(1-adamantyl)-2-methylphenol

생성물 1

HCID 86729430HCID 86729430, 화합물수율 95.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-(adamantan-1-yl)-2-methylphenol (2.0 g, 8.76 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (3.63 g, 23.29 mmol) and ethyl chloroacetate (1.29 g, 10.51 mmol), and stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with aqueous sodium bicarbonate. The organic layer was dried over anhydrous magnesium sulfate. The solvent was filtered and evaporated under reduced pressure to afford a crude solid, which was purified by silica gel column chromatography to give ethyl 2-(4-(adamantan-1-yl)-2-methylphenoxy)acetate as a white solid (2.6 g, 95.9% yield).

후처리

  1. washwashed with aqueous sodium bicarbonate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationThe solvent was filtered
  4. customevaporated under reduced pressure
  5. customto afford a crude solid, which
  6. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-3a2eac7df19649cdbb8266b40ac564e5
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315507B2

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