[2-(6-Methoxy-quinazolin-4-yl)-ethyl]-1,4-dioxa-spiro[4.5]decan-8-ol → 4-Hydroxy-4-[2-(6-methoxyquinazolin-4-yl)-ethyl]cyclohexanone

HRID 1354207노트

반응식

HRID 1354207 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][N:7]=[C:6]2[CH2:13][CH2:14][CH:15]1[CH2:19]OC2(CCC(O)CC2)[O:16]1>CC(O)=O.C1COCC1.O>[OH:16][C:15]1([CH2:14][CH2:13][C:6]2[C:5]3[C:10](=[CH:11][CH:12]=[C:3]([O:2][CH3:1])[CH:4]=3)[N:9]=[CH:8][N:7]=2)[CH2:19][CH2:4][C:3](=[O:2])[CH2:12][CH2:11]1

참가 물질

3

실험 절차

A solution of 8-([2-(6-methoxy-quinazolin-4-yl)-ethyl]-1,4-dioxa-spiro[4.5]decan-8-ol (0.623 g, 1.81 mmol) in AcOH/THF/H2O (3/2/2, 10 ml) was stirred at 60° C. for 30 hours. The reaction mixture was concentrated to dryness by rotary evaporation. The residue was diluted with sodium bicarbonate (100 ml) and ethyl acetate (100 ml), the phases were separated and the aqueous phase was extracted twice using 50 ml of ethyl acetate each time. The combined organic phases were dried over MgSO4, filtered and concentrated to dryness by rotary evaporation.

후처리

  1. concentrationThe reaction mixture was concentrated to dryness by rotary evaporation
  2. additionThe residue was diluted with sodium bicarbonate (100 ml) and ethyl acetate (100 ml)
  3. customthe phases were separated
  4. extractionthe aqueous phase was extracted twice
  5. dry with materialThe combined organic phases were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated to dryness by rotary evaporation

출처 및 근거

ORD 기록
ord-c20cf818732b4141af723199b7b09873
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223776B2

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