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Chlorotrimethylsilane → Ethyl 3-(benzyl(3-ethoxy-3-oxopropyl)amino)-2,2-difluoropropanoate

HRID 451556
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HRID 451556 반응식
[Si](Cl)(C)(C)C.Br[C:7]([F:14])([F:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9].[CH2:15]([O:17][C:18](=[O:39])[CH2:19][CH2:20][N:21]([CH2:29]N1C2C=CC=CC=2N=N1)[CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH3:16].C([O-])(O)=O.[Na+]>C1COCC1.[Zn]>[CH2:22]([N:21]([CH2:20][CH2:19][C:18]([O:17][CH2:15][CH3:16])=[O:39])[CH2:29][C:7]([F:14])([F:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
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참가 물질

7

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 69585Ethyl bromodifluoroacetateHCID 516892Sodium BicarbonateHCID 594427333-(Benzotriazol-1-ylmethylbenzylamino)propionic acid ethyl ester

생성물 1

HCID 59442745Ethyl 3-(benzyl(3-ethoxy-3-oxopropyl)amino)-2,2-difluoropropanoate수율 99.4%

시약·촉매·용매 2

HCID 23994
Zinc
촉매
HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of activated zinc dust (4.13 g, 63.2 mmol) in dry THF (100 mL) under argon was added TMS-Cl (3.60 g, 4.24 mL, 33.2 mmol). After 10 minutes ethyl bromodifluoroacetate (7.05 g, 4.49 mL, 34.7 mmol) was added slowly, whereby the temperature was kept below 30° C. (cooling with a waterbath). Then a solution of 3-(benzotriazol-1-ylmethyl-benzyl-amino)-propionic acid ethyl ester (10.69 g, 31.6 mmol) in dry THF (100 mL) was added. The exothermic reaction was kept between 20 and 25° C. with a waterbath. The reaction mixture was stirred at room temperature for 12 hours. The reaction mixture was poured on 5% aqueous NaHCO3 solution and filtered over dicalite. The filtrate was extracted three times with ethyl acetate. The organic layers were washed with water and 1 N HCl, then dried over Na2SO4, filtered and the solvents were evaporated. The residue was purified by flash chromatography (silica gel, 100 g, 0% to 50% EtOAc in heptane) to give the title compound as colorless liquid (10.78 g, 99%).

후처리

  1. customwas kept below 30° C.
  2. temperaturecooling with a waterbath)
  3. customThe exothermic reaction
  4. customwas kept between 20 and 25° C. with a waterbath
  5. filtrationfiltered over dicalite
  6. extractionThe filtrate was extracted three times with ethyl acetate
  7. washThe organic layers were washed with water and 1 N HCl
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. customthe solvents were evaporated
  11. customThe residue was purified by flash chromatography (silica gel, 100 g, 0% to 50% EtOAc in heptane)

출처 및 근거

ORD 기록
ord-3382ecc366394f04b9c4a8799eb5972f
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486967B2

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