[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 1354207ノート

反応式

HRID 1354207 の反応式
[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

参加物

3

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c20cf818732b4141af723199b7b09873
出典データセット
uspto-grants-2007_05
特許番号
US07223776B2

反応ノート

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