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

Methyl iodide → Methyl (2s)-2-[(3r)-3-(n-[tert-butyloxycarbonyl]amino)-2-oxo-pyrrolidin-1-yl]propionate

HRID 2288054
노트
인쇄 미리보기

반응식

HRID 2288054 반응식
CI.[NH:3]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C@@H:4]([C:9]([NH:11][C@H:12]([C:14]([O:16][CH3:17])=[O:15])[CH3:13])=[O:10])[CH2:5][CH2:6]SC>CN(C=O)C.ClCCl>[C:21]([O:20][C:18]([NH:3][C@@H:4]1[CH2:5][CH2:6][N:11]([C@@H:12]([CH3:13])[C:14]([O:16][CH3:17])=[O:15])[C:9]1=[O:10])=[O:19])([CH3:24])([CH3:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6328Methyl iodideHCID 11024115Boc-(D)-Met-(L)-Ala-OMe

생성물 1

HCID 9838823Methyl (2s)-2-[(3r)-3-(n-[tert-butyloxycarbonyl]amino)-2-oxo-pyrrolidin-1-yl]propionate수율 61.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

Methyl iodide (10 ml) was added to Boc-(D)-Met-(L)-Ala-OMe (8 g) in a mixture of DMF (20 ml) and dichloromethane (20 ml) and the mixture was allowed to stand for 16 hours and then evaporated to dryness. Further dichloromethane (2×50 ml) was added and evaporated to remove residual methyl iodide and the residue was dissolved in a mixture of DMF (300 ml) and dichloromethane (300 ml). The mixture was cooled to ~5° C. and sodium Wydride (0.76 g of an 80% dispersion in mineral oil) was add ed in one portion and the mixture was stirred at this temperature for 2 hours. Saturated aqueous ammonium chloride (50 ml) was added and the mixture was evaporated to dryness and then partitioned between water and ether. The ether extract was washed with brine and dried and evaporated to give a gum which was purified by flash chromatography on a sinter flinnel (25% ethyl acetate:hexane to 100% ethylacetate) to give methyl (2S)-2-[(3R)-3-(N-[tert-butyloxycarbonyl]amino)-2-oxo-pyrrolidin-1-yl]propionate as a gum (4.2 g) which crystallised on standing: NMR (CDCl3): 1.4 (s, 9H), 1.4 (d, 3H), 1.8 (m, 1H), 2.6 (m, 1H), 3.4 (m, 2H), 3.7 (m, 3H), 4.2 (m, 1H), 4.9 (q, 1H), 5.2 (bs, 1H).

후처리

  1. customevaporated to dryness
  2. additionFurther dichloromethane (2×50 ml) was added
  3. customevaporated
  4. customto remove residual methyl iodide
  5. dissolutionthe residue was dissolved in a mixture of DMF (300 ml) and dichloromethane (300 ml)
  6. temperatureThe mixture was cooled to ~5° C.
  7. additionsodium Wydride (0.76 g of an 80% dispersion in mineral oil) was add
  8. additionSaturated aqueous ammonium chloride (50 ml) was added
  9. customthe mixture was evaporated to dryness
  10. custompartitioned between water and ether
  11. extractionThe ether extract
  12. washwas washed with brine
  13. customdried
  14. customevaporated
  15. customto give a gum which
  16. customwas purified by flash chromatography on a sinter flinnel (25% ethyl acetate:hexane to 100% ethylacetate)

출처 및 근거

ORD 기록
ord-66b2375c7deb40a0bc84da0f2b9461e8
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06087336

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트