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Hydrochloric Acid → (R)-N-[(1R,2R)-3-[[(1,1-Dimethylethyl)diphenylsilyl]oxy]-2-methyl-1-phenylpropyl]-2-methyl-2-propanesulfinamide

HRID 1697309
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HRID 1697309 반응식
[H-].C([Al+]CC(C)C)C(C)C.[CH3:11][C:12]([Si:15]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[O:16][CH2:17][C@H:18]([CH3:25])[C:19]([N:21](OC)C)=O)([CH3:14])[CH3:13].Cl.[CH3:39][C:40]([S@:43](N)=[O:44])([CH3:42])[CH3:41].[C:46]1([Mg]Br)[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1>O1CCCC1.C(OCC)(=O)C.ClCCl.C(OCC)C.[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC>[CH3:11][C:12]([Si:15]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)[O:16][CH2:17][C@H:18]([CH3:25])[C@@H:19]([NH:21][S@@:43]([C:40]([CH3:42])([CH3:41])[CH3:39])=[O:44])[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)([CH3:14])[CH3:13]
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참가 물질

11

반응물 5

HCID 313Hydrochloric AcidHCID 10964479tert-Butylsulfinamide, (R)-(+)-HCID 21225700DiisobutylaluminumhydrideHCID 86663240(2S)-3-[[(1,1-Dimethylethyl)diphenylsilyl]oxy]-N-methoxy-N,2-dimethyl-propanamideHCID 178418255HCID 178418255, 화합물

생성물 1

HCID 66690258
(R)-N-[(1R,2R)-3-[[(1,1-Dimethylethyl)diphenylsilyl]oxy]-2-methyl-1-phenylpropyl]-2-methyl-2-propanesulfinamide

시약·촉매·용매 5

HCID 76524Titanium tetraethoxide촉매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매3회HCID 8857Ethyl Acetate용매2회

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온도
-50 °C

실험 절차

A solution of diisobutylaluminium hydride in tetrahydrofuran (1M, 50 mL) was added dropwise to a stirred solution of (2S)-3-[[(1,1-dimethylethyl)diphenylsilyl]oxy]-N-methoxy-N,2-dimethyl-propanamide (Example 136a, 6.2 g) in tetrahydrofuran (40 mL) at 0° C. The mixture was stirred for 30 minutes and poured onto a mixture of ethyl acetate (250 mL) and 2M hydrochloric acid (100 mL). The organic phase was washed with brine, dried (Na2SO4), filtered and concentrated in vacuo to give the crude aldehyde. Tetrahydrofuran (30 mL) was added followed by (R)-(+)-2-methyl-2-propanesulfinamide (2.6 g) and titanium ethoxide (10 mL). The mixture was stirred at room temperature for 90 min., then diluted with ethyl acetate (300 mL) and quenched with brine (100 mL). The mixture was stirred for 1 h. The organic phase was separated, dried (Na2SO4), filtered through a pad of Celite and concentrated in vacuo to give the crude sulfinimine, which was dissolved in dry dichloromethane (90 mL) and the solution was cooled to −50° C. A solution of phenylmagnesium bromide in diethyl ether (3M, 13 mL) was added dropwise and the reaction mixture was warmed up to 0° C. over 3 h, quenched with sat. aqueous NH4Cl (150 mL) and extracted into dichloromethane. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified (SiO2 chromatography eluting with iso-hexane:ethyl acetate (0-100%)) to give the subtitle compound (5.2 g).

후처리

  1. washThe organic phase was washed with brine
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto give the crude aldehyde
  6. stirringThe mixture was stirred at room temperature for 90 min.
  7. customquenched with brine (100 mL)
  8. stirringThe mixture was stirred for 1 h
  9. customThe organic phase was separated
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered through a pad of Celite
  12. concentrationconcentrated in vacuo
  13. customto give the crude sulfinimine, which
  14. temperaturethe reaction mixture was warmed up to 0° C. over 3 h
  15. customquenched with sat. aqueous NH4Cl (150 mL)
  16. extractionextracted into dichloromethane
  17. dry with materialThe organic phase was dried (Na2SO4)
  18. filtrationfiltered
  19. concentrationconcentrated in vacuo
  20. customThe residue was purified
  21. wash(SiO2 chromatography eluting with iso-hexane:ethyl acetate (0-100%))

출처 및 근거

ORD 기록
ord-cd92b69e24234f76830acb39f08fff11
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163905B2

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