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Water → N-cyclopropyl-3-[6-(2,3-dihydroxy-2-methylpropoxy)-4-oxoquinazolin-3(4H)-yl]-4-methylbenzamide

HRID 2354206
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HRID 2354206 반응식
[CH:1]1([NH:4][C:5](=[O:29])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([N:13]3[C:22](=[O:23])[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([O:24][CH2:25][C:26]([CH3:28])=[CH2:27])[CH:20]=4)[N:15]=[CH:14]3)[CH:7]=2)[CH2:3][CH2:2]1.C[N+]1([O-])CCOCC1.S(=O)(O)[O-].[Na+].[OH2:43].CC(C)=O.[OH2:48]>CC(O)(C)C.[Os](=O)(=O)(=O)=O>[CH:1]1([NH:4][C:5](=[O:29])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([N:13]3[C:22](=[O:23])[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([O:24][CH2:25][C:26]([OH:48])([CH3:28])[CH2:27][OH:43])[CH:20]=4)[N:15]=[CH:14]3)[CH:7]=2)[CH2:3][CH2:2]1
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참가 물질

8

반응물 5

HCID 962WaterHCID 82029Methyl morpholine oxideHCID 18366337Propan-2-one--water (1/1)HCID 23665763Sodium BisulfiteHCID 66918821HCID 66918821, 화합물

생성물 1

HCID 11774562N-cyclopropyl-3-[6-(2,3-dihydroxy-2-methylpropoxy)-4-oxoquinazolin-3(4H)-yl]-4-methylbenzamide

시약·촉매·용매

2
HCID 30318Osmium Tetroxide촉매HCID 6386tert-Butanol용매

실험 절차

To a solution of N-cyclopropyl-4-methyl-3-[6-[(2-methylprop-2-en-1-yl)oxy]-4-oxoquinazolin-3(4H)-yl]benzamide (1.76 g) in acetone/water (4:1, 40 ml) was added N-methylmorpholine-N-oxide (2.1 g) followed by a solution of osmium tetroxide in 2-methyl-2-propanol (2.5% solution, 1.2 ml). After 18 hours sodium bisulfite (0.1 g) was added and the mixture stirred for a further 1 hour. The crude mixture was poured into water (20 ml) and extracted into ethyl acetate (300 ml). The combined organic extracts were washed with brine (100 ml), dried (magnesium sulfate) and concentrated. Purification by preparative HPLC provided N-cyclopropyl-3-[6-(2,3-dihydroxy-2-methylpropoxy)-4-oxoquinazolin-3(4H)-yl]4 methylbenzamide (AZ12197886) (0.5 g); NMR Spectrum: (CDCl3) 0.45 (m, 2H), 0.75 (m, 2H), 1.32 (s, 3H), 1.70 (m, 2H), 2.10 (s, 3H), 2.70 (m, 1H), 3.60 (d, 1H), 3.70 (m, 1H), 3.90 (m, 2H), 6.70 (d, 1H), 7.30 (m, 1H), 7.45 (m, 1H), 7.50 (m, 2H), 7.70 (m, 1H), 7.90 (s, 1H), 7.95 (t, 1H); Mass Spectrum: M+H+ 424. Further elution provided N-cyclopropyl-3-(6-isobutoxy-4-oxoquinazolin-3(4H)-yl)-4-methylbenzamide (AZ12198379) as a clear oil (70 mg); NMR Spectrum (CDCl3) 0.50 (m, 2H), 0.90 (m, 2H), 1.10 (s, 3H), 1.15 (s, 3H), 2.15 (m, 1H), 2.20 (s, 3H), 2.90 (m, 1H), 3.90 (d, 2H), 6.60 (s, 1H), 7.40 (m, 2H), 7.60 (d, 1H), 7.70 (m, 2H), 7.80 (m, 1H), 7.90 (s, 1H); Mass Spectrum M+H+ 392.

후처리

  1. extractionextracted into ethyl acetate (300 ml)
  2. washThe combined organic extracts were washed with brine (100 ml)
  3. dry with materialdried (magnesium sulfate)
  4. concentrationconcentrated
  5. customPurification by preparative HPLC

출처 및 근거

ORD 기록
ord-4cbe3e6d15f34ad0918c92f65ef5f7e8
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07750154B2

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