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L-Threonine → Ethyl5-((1R)-1-{[(R)-tert-butylsulfinyl]amino}ethyl)-2-[(methylsulfonyl)amino]benzoate

HRID 230590
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HRID 230590 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[C:8]([CH:13]=1)[C:9]([O:11][CH3:12])=[O:10])(=O)[CH3:2].[CH3:19][C:20]([S@:23]([NH2:25])=[O:24])([CH3:22])[CH3:21].[BH4-].[Na+].[CH3:28][C@@H](O)[C@H](N)C(O)=O>[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC.O1CCCC1>[CH2:12]([O:11][C:9](=[O:10])[C:8]1[CH:13]=[C:4]([C@H:1]([NH:25][S@@:23]([C:20]([CH3:22])([CH3:21])[CH3:19])=[O:24])[CH3:2])[CH:5]=[CH:6][C:7]=1[NH:14][S:15]([CH3:18])(=[O:17])=[O:16])[CH3:28]
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참가 물질

7

반응물 4

HCID 6288L-ThreonineHCID 4311764Sodium borohydrideHCID 10964479tert-Butylsulfinamide, (R)-(+)-HCID 66978055Methyl 5-acetyl-2-[(methylsulfonyl)amino]benzoate

생성물 1

HCID 57762930Ethyl5-((1R)-1-{[(R)-tert-butylsulfinyl]amino}ethyl)-2-[(methylsulfonyl)amino]benzoate수율 23%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 76524Titanium tetraethoxide용매

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온도
80 °C

실험 절차

To a mixture of methyl 5-acetyl-2-[(methylsulfonyl)amino]benzoate (13.2 g, 49 mmol, PCT Int. Appl. WO2005003084) in titanium (IV) ethoxide (100 ml) and tetrahydrofuran (THF) (100 ml) was added (R)-(+)-2-methylpropane-2-sulfinamide (5.9 g, 49 mmol, Advanced Asymmmetry) and the mixture was stirred for 16 hours at 80° C. The mixture was cooled to room temperature and then to 0° C. before it was added dropwise into a 0° C. solution of sodium borohydride (7.4 g, 195 mmol). Thre mixture was stirred at 0° C. for 3 hours and then warmed to room temperature. The reaction was quenched with methanol and stirred for 30 minutes. Water was added to the mixture and it was stirred for 10 minutes. The resulting suspension was filtered through a pad of Celite and the filter cake was washed with ethyl acetate. The filtrate was concentrated under reduced pressure to give the residue, which was applied to a silica gel chromatography column and eluted with a volume mixture of dichloromethane and ethyl acetate (1:1) to furnish 4.3 g (23% yield) of the title compound as a slightly yellow solid.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. temperaturewarmed to room temperature
  3. customThe reaction was quenched with methanol
  4. stirringstirred for 30 minutes
  5. additionWater was added to the mixture and it
  6. stirringwas stirred for 10 minutes
  7. filtrationThe resulting suspension was filtered through a pad of Celite
  8. washthe filter cake was washed with ethyl acetate
  9. concentrationThe filtrate was concentrated under reduced pressure
  10. customto give the residue, which
  11. washeluted with a volume mixture of dichloromethane and ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-495160335735484182ccb75216961d8a
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07566739B2

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