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Potassium Carbonate → Methyl 3-[(4-methyl-5-oxo-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-9-yl)oxy]-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate

HRID 600559
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반응식

HRID 600559 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]2[CH2:17][CH2:16][N:15]([CH3:18])[C:14]2=[O:19])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].F[C:21]1[CH:30]=[C:29]2[C:24]([C:25](=[O:32])[N:26]([CH3:31])[CH2:27][O:28]2)=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:31][N:26]1[C:25](=[O:32])[C:24]2[C:29](=[CH:30][C:21]([O:1][C:2]3[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]4[CH2:17][CH2:16][N:15]([CH3:18])[C:14]4=[O:19])[CH:11]=3)[C:5]([O:7][CH3:8])=[O:6])=[CH:22][CH:23]=2)[O:28][CH2:27]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 576631937-Fluoro-3-methyl-2,3-dihydro-4H-1,3-benzoxazin-4-oneHCID 59761136methyl 3-hydroxy-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate2회

생성물 1

HCID 59761137Methyl 3-[(4-methyl-5-oxo-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-9-yl)oxy]-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate수율 54%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

실험 절차

A mixture of methyl 3-hydroxy-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate (Intermediate 8) (0.27 g, 1 mmol), 9-fluoro-4-methyl-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-5-one (CAS no. 915771-24-3) (200 mg, 11 mol) and potassium carbonate (276 g, 2 mmol) in acetonitrile (20 mL) was heated in a microwave at 160° C. for 12 hours. The mixture was evaporated and the residue partitioned between ethyl acetate (40 mL) and water (40 mL). The organic phase was separated, washed with water (10 mL) and brine (20 mL), dried (MgSO4) and evaporated. The aqueous phase was acidified to pH 1 with 2N hydrochloric acid extracted with ethyl acetate (2×30 mL). The combined organic extracts were washed with water (2×20 mL), brine (20 mL), dried (MgSO4) and evaporated. The residue was dissolved in THF (2 mL) and methanol (1 mL) and treated with 2M TMS-diazomethane (0.14 mL) stirred for 30 minutes. The mixture was evaporated and the residue combined with that from the initial extraction and purified by flash chromatography on silica eluting with 0 to 100% ethyl acetate in isohexane to afford the product (232 mg, 54%). 1H NMR δ (300 MHz, CDCl3) 2.10-2.25 (m, 1H), 2.53-2.66 (m, 1H), 2.93 (s, 3H), 3.09 (s, 3H), 3.32-3.58 (m, 2H), 3.89 (s, 3H), 4.91 (t, 1H), 5.17 (s, 2H), 6.51 (s, 1H), 6.72 (d, 1H), 6.97 (s, 1H), 7.34 (s, 1H), 7.52 (s, 1H), 7.93 (d, 1H); m/z 427 (M+H+).

후처리

  1. customThe mixture was evaporated
  2. customthe residue partitioned between ethyl acetate (40 mL) and water (40 mL)
  3. customThe organic phase was separated
  4. washwashed with water (10 mL) and brine (20 mL)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. extractionextracted with ethyl acetate (2×30 mL)
  8. washThe combined organic extracts were washed with water (2×20 mL), brine (20 mL)
  9. dry with materialdried (MgSO4)
  10. customevaporated
  11. dissolutionThe residue was dissolved in THF (2 mL)
  12. additionmethanol (1 mL) and treated with 2M TMS-diazomethane (0.14 mL)
  13. customThe mixture was evaporated
  14. extractionextraction
  15. custompurified by flash chromatography on silica eluting with 0 to 100% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-f05471954af94f27809b81899bc4ee09
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902200B2

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