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

HRID 57504
ノート
印刷プレビュー

反応式

HRID 57504 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 67553
Tetrabutylammonium Iodide
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eeb454d1dc75494693aa19eccfa8f2f4
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434719B2

反応ノート

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