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Bicarbonate Ion → N-(7-bromo-3-chloro-1-fluoro-5H-chromeno[2,3-c]pyridin-5-ylidene)-2-methylpropane-2-sulfinamide

HRID 1409504
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HRID 1409504 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:15](=[CH:16][CH:17]=1)[O:14][C:7]1[C:8]([F:13])=[N:9][C:10]([Cl:12])=[CH:11][C:6]=1[C:5]2=O.[CH3:19][C:20]([S:23]([NH2:25])=[O:24])([CH3:22])[CH3:21].C(=O)(O)[O-]>C1COCC1.[Cl-].[Na+].O.C(O[Ti](OCC)(OCC)OCC)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:15](=[CH:16][CH:17]=1)[O:14][C:7]1[C:8]([F:13])=[N:9][C:10]([Cl:12])=[CH:11][C:6]=1[C:5]2=[N:25][S:23]([C:20]([CH3:22])([CH3:21])[CH3:19])=[O:24]
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참가 물질

7

반응물 3

HCID 769Bicarbonate IonHCID 3382465Tert-ButanesulfinamideHCID 574756427-bromo-3-chloro-1-fluoro-5H-chromeno[2,3-c]pyridin-5-one

생성물 1

HCID 86658361N-(7-bromo-3-chloro-1-fluoro-5H-chromeno[2,3-c]pyridin-5-ylidene)-2-methylpropane-2-sulfinamide

시약·촉매·용매 3

HCID 178477244HCID 178477244, 화합물촉매
HCID 8028
Tetrahydrofuran
용매
HCID 57417360Sodium chloride; water용매

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온도
75 °C

실험 절차

A mixture of 7-bromo-3-chloro-1-fluoro-5H-chromeno[2,3-c]pyridin-5-one (740 mg, 2.25 mmol, Example 4), 2-methyl-2-propane-sulfinamide (819 mg, 6.76 mmol, Aldrich), and tetraethoxytitanium (6.07 mL, 29.3 mmol, Aldrich) in dry THF (15 mL) was heated at 75° C. for 24 hours under nitrogen atmosphere. The mixture was cooled to RT and brine and aqueous, saturated bicarbonate solution were added while rapidly stirring. After 1 h, the resulting suspension was filtered through celite, and the filter cake was washed with EtOAc. The filtrate was washed with brine and dried over MgSO4. The solvent was removed under reduced pressure and the remaining residue was purified by flash chromatography on silica gel (0-20% EtOAc/hexanes) to afford the title product as an orange solid. MS m/z=423.8 [M+H]+. Calculated for C16H13BrClFN2O2S: 431.71.

후처리

  1. temperatureThe mixture was cooled to RT
  2. filtrationthe resulting suspension was filtered through celite
  3. washthe filter cake was washed with EtOAc
  4. washThe filtrate was washed with brine
  5. dry with materialdried over MgSO4
  6. customThe solvent was removed under reduced pressure
  7. customthe remaining residue was purified by flash chromatography on silica gel (0-20% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-fcb6cadf3c334ff8a362511143d243b7
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921363B2

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