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P-Chloroacetophenone → Methyl {1-[1-(4-chlorophenyl)ethyl]azetidin-3-ylidene}(3,5-difluorophenyl)acetate

HRID 602671
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HRID 602671 반응식
[NH:1]1[CH2:4][C:3](=[C:5]([C:10]2[CH:15]=[C:14]([F:16])[CH:13]=[C:12]([F:17])[CH:11]=2)[C:6]([O:8][CH3:9])=[O:7])[CH2:2]1.[CH3:18][C:19]([C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1)=O.C(N(CC)CC)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C>[Cl:27][C:24]1[CH:25]=[CH:26][C:21]([CH:19]([N:1]2[CH2:4][C:3](=[C:5]([C:10]3[CH:15]=[C:14]([F:16])[CH:13]=[C:12]([F:17])[CH:11]=3)[C:6]([O:8][CH3:9])=[O:7])[CH2:2]2)[CH3:18])=[CH:22][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7467P-ChloroacetophenoneHCID 8471TriethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 67065925Methyl azetidin-3-ylidene(3,5-difluorophenyl)acetate

생성물 1

HCID 67065932Methyl {1-[1-(4-chlorophenyl)ethyl]azetidin-3-ylidene}(3,5-difluorophenyl)acetate

시약·촉매·용매 1

HCID 6365
1,1-Dichloroethane
용매

실험 절차

A solution of 0.142 g (0.5 mmole) of methyl azetidin-3-ylidene(3,5-difluorophenyl)acetate, 0.142 g (1 mmol) of 4-chloroacetophenone and 0.15 mL (12 mmol) of triethylamine in 5 mL of dichloroethane was stirred at room temperature. After 5 min, 0.422 g (2 mmol) of sodium triacetoxyborohydride was added and the mixture was stirred at room temperature for 3 h. The reaction was quenched by addition of saturated KHCO3 solution and the mixture was partitioned between 10 mL ether and 2 mL saturated KHCO3 solution. The layers were separated and the organic layer was dried over Na2SO4, and concentrated. The residue was purified by reverse phase chromatography (Waters Xterra C18, 19 mm×10 mm) using a gradient of CH3CN—H2O-Et3N (20:80:0.1 to 60:40:0.1) to afford the title compound; Mass Spectrum: m/e=378 (M+1 35Cl) and 380 (M+1 35Cl).

후처리

  1. customThe reaction was quenched by addition of saturated KHCO3 solution
  2. customthe mixture was partitioned between 10 mL ether and 2 mL saturated KHCO3 solution
  3. customThe layers were separated
  4. dry with materialthe organic layer was dried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by reverse phase chromatography (Waters Xterra C18, 19 mm×10 mm)

출처 및 근거

ORD 기록
ord-0de440b1db484c91a738633f6dce88c8
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07906503B2

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