홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethyl Propionate → (S)-2-(2-Oxo-2H-pyrid-1-yl)-propionic acid ethyl ester

HRID 602919
노트
인쇄 미리보기

반응식

HRID 602919 반응식
[NH:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]1=[O:7].[H-].[Na+].[CH2:10]([O:12][C:13](=[O:16])[CH2:14][CH3:15])[CH3:11]>C1COCC1>[CH2:10]([O:12][C:13](=[O:16])[C@@H:14]([N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]1=[O:7])[CH3:15])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7749Ethyl PropionateHCID 88712-PyridoneHCID 24758Sodium hydride

생성물 1

HCID 66650045(S)-2-(2-Oxo-2H-pyrid-1-yl)-propionic acid ethyl ester수율 46.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A stirred solution of 1H-Pyridin-2-one (500 mg, 5.26 mmol) in anhydrous THF (50 ml) at room temperature was treated portionwise with 60% NaH (231 mg, 5.78 mmol). The reaction mixture was kept for 10 min then added over 5 min to a solution of (R)-2-trifluoromethanesulfonyloxy)-propionic acid ethyl ester (1315 mg, 5.26 mmol) in anhydrous THF (2.5 ml) at room temperature. The resulting mixture was stirred for 2 h, then concentrated. The residue was dissolved in ethyl acetate, and the resulting solution was washed with ice cold dilute HCl. The organic layer was removed and the aqueous layer re-extracted with ethyl acetate. The combined organic extracts were dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography (20% up to 80% ethyl acetate in hexane) to afford the title compound as a yellow oil (480 mg, 46%): [α]27D=−56.4° (c=0.275, CH2Cl2); 1H NMR (400 MHz CDCl3) δ 1.3 (3H, t), 1.65 (3H, d), 4.2 (2H, q), 5.6 (1H, q), 6.2 (1H, t), 6.4 (1H, d), 7.2-7.3 (2H, m).

후처리

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washthe resulting solution was washed with ice cold dilute HCl
  4. customThe organic layer was removed
  5. extractionthe aqueous layer re-extracted with ethyl acetate
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography (20% up to 80% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-ead1519f8bbb4c039e3fd665ac4f08e8
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07906650B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트