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

Iodine → diethyl[(4R,9aS)-6-oxo-4-(3,4,5-trifluorophenyl)octahydropyrido[2,1-c][1,4]oxazin-7-yl]phosphonate

HRID 16351
노트
인쇄 미리보기

반응식

HRID 16351 반응식
[I-].[F:2][C:3]1[CH:4]=[C:5]([C@@H:11]2[CH2:16][O:15][CH2:14][C@@H:13]3[CH2:17][CH2:18][CH2:19][C:20](=[O:21])[N:12]23)[CH:6]=[C:7]([F:10])[C:8]=1[F:9].CN(C)CCN(C)C.II.S([O-])([O-])(=O)=S.[Na+].[Na+].[P:39]([O:46]CC)([O:43][CH2:44][CH3:45])[O:40][CH2:41][CH3:42]>C(OCC)(=O)C.C(Cl)Cl>[CH2:41]([O:40][P:39]([CH:19]1[C:20](=[O:21])[N:12]2[C@H:13]([CH2:14][O:15][CH2:16][C@H:11]2[C:5]2[CH:6]=[C:7]([F:10])[C:8]([F:9])=[C:3]([F:2])[CH:4]=2)[CH2:17][CH2:18]1)(=[O:46])[O:43][CH2:44][CH3:45])[CH3:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 807IodineHCID 8037N,N,N',N'-TetramethylethylenediamineHCID 24477Sodium ThiosulfateHCID 30165Iodide IonHCID 31215Triethyl phosphiteHCID 44124045(4R,9aS)-4-(3,4,5-Trifluorophenyl)hexahydropyrido[2,1-c][1,4]oxazin-6(1H)-one

생성물 1

HCID 86612713
diethyl[(4R,9aS)-6-oxo-4-(3,4,5-trifluorophenyl)octahydropyrido[2,1-c][1,4]oxazin-7-yl]phosphonate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

In nitrogen atmosphere, trimethylsilyle iodide (0.188 mL) was added to a methylene chloride solution (6 mL) of (4R,9aS)-4-(3,4,5-trifluorophenyl)hexahydropyrido[2,1-c][1,4]oxazin-6-one (252 mg) and N,N,N′,N′-tetramethylethylenediamine (0.466 mL) at 0° C. The resulting reaction solution was stirred under ice-cooling for 30 min, and iodine (336 mg) was added thereto under ice-cooling. The resulting reaction solution was stirred under ice-cooling for 1 hr, and ethyl acetate and a saturated sodium thiosulfate aqueous solution were added thereto. The organic layer was separated, washed with saturated saline, dried over magnesium sulfate, and concentrated under reduced pressure to give a crude iodinated substance. To the given crude iodinated substance, triethyl phosphite (3 mL) was added. The resulting mixture was stirred at 120° C. for 2 hr, allowed to cool to room temperature, and then concentrated under reduced pressure to give 372 mg of the title compound. The physical property values of this compound were as follows:

후처리

  1. customThe resulting reaction solution
  2. temperaturecooling for 30 min
  3. temperatureunder ice-cooling
  4. customThe resulting reaction solution
  5. stirringwas stirred under ice-
  6. temperaturecooling for 1 hr
  7. customThe organic layer was separated
  8. washwashed with saturated saline
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customto give a crude
  12. additionwas added
  13. stirringThe resulting mixture was stirred at 120° C. for 2 hr
  14. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b821cd62ac954a23a425bea5b716d3b4
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737141B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트