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Ethyl Acetate → (R)-4-[(R)-1-(tert-Butoxy)ethyl]-3-(4-methoxybenzyl)oxazolidin-2-one

HRID 57504
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HRID 57504 반응식
C([O:8][C:9](=[O:21])[NH:10][C@@H:11]([C@H:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH3:15])[CH2:12]O)C1C=CC=CC=1.[H-].[Na+].[CH3:24][O:25][C:26]1[CH:33]=[CH:32][C:29]([CH2:30]Cl)=[CH:28][CH:27]=1.CCOC(C)=O>CN(C=O)C.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:17]([O:16][C@@H:14]([C@H:11]1[CH2:12][O:21][C:9](=[O:8])[N:10]1[CH2:30][C:29]1[CH:32]=[CH:33][C:26]([O:25][CH3:24])=[CH:27][CH:28]=1)[CH3:15])([CH3:18])([CH3:19])[CH3:20]
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참가 물질

7

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HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 699934-Methyloxybenzyl chlorideHCID 59113072benzyl ((2R,3R)-3-(tert-butoxy)-1-hydroxybutan-2-yl)carbamate

생성물 1

HCID 90422856(R)-4-[(R)-1-(tert-Butoxy)ethyl]-3-(4-methoxybenzyl)oxazolidin-2-one수율 96.5%

시약·촉매·용매 2

HCID 67553
Tetrabutylammonium Iodide
촉매
HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

To a solution of benzyl((2R,3R)-3-(tert-butoxy)-1-hydroxybutan-2-yl)carbamate (5.88 g, 19.9 mmol) in 100 mL DMF was added NaH (60% in mineral oil, 1.62 g, 40.6 mmol) at 0° C. The reaction mixture was stirred for 30 min at 0° C. To the reaction mixture were added 4-methoxybenzyl chloride (4.07 mL, 29.9 mmol) and tetrabutylammonium iodide (0.74 g, 1.99 mmol) and the resulting mixture was warmed to room temperature and stirred for 15.5 h. The reaction mixture was poured into ice water (200 mL) forming a white suspension. EtOAc (100 mL) was added and the resulting mixture was stirred for 5 min to form a clear two layer solution. After separation, the aqueous phase was extracted with EtOAc (100 mL×3). The combined organic solution was washed with brine (80 mL), dried over Na2SO4, filtered and concentrated. Flash column chromatography (EtOAc/Heptane 0 to 70%) gave 5.90 g of (R)-4-((R)-1-(tert-butoxy)ethyl)-3-(4-methoxybenzyl)oxazolidin-2-one with minor impurities. Major product 1H NMR (400 MHz, MeOD) δ 7.38-7.29 (m, 2H), 6.99-6.93 (m, 2H), 4.68-4.58 (m, 1H), 4.33 (dd, J=9.3, 4.5 Hz, 1H), 4.27-4.17 (m, 2H), 3.89 (dd, J=6.4, 4.8 Hz, 1H), 3.81 (s, 3H), 3.65 (dd, J=9.0, 4.6 Hz, 1H), 1.09 (s, 9H), 1.02 (d, J=6.3 Hz, 3H). MS m/z 308.2 (M+H).

후처리

  1. temperaturethe resulting mixture was warmed to room temperature
  2. stirringstirred for 15.5 h
  3. customforming a white suspension
  4. stirringthe resulting mixture was stirred for 5 min
  5. customto form a clear two layer solution
  6. customAfter separation
  7. extractionthe aqueous phase was extracted with EtOAc (100 mL×3)
  8. washThe combined organic solution was washed with brine (80 mL)
  9. dry with materialdried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-eeb454d1dc75494693aa19eccfa8f2f4
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434719B2

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