Diphenylmethane → Methyl azetidin-3-yl(3,5-difluorophenyl)acetate

HRID 1724188노트

반응식

HRID 1724188 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9](=[C:14]2[CH2:17][N:16](C(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:15]2)[C:10]([O:12][CH3:13])=[O:11])[CH:5]=[C:6]([F:8])[CH:7]=1.C1(CC2C=CC=CC=2)C=CC=CC=1>CO.Cl.CCOCC.[Pd]>[NH:16]1[CH2:17][CH:14]([CH:9]([C:4]2[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[CH:3]=2)[C:10]([O:12][CH3:13])=[O:11])[CH2:15]1

참가 물질

7

반응물 2

HCID 7580DiphenylmethaneHCID 57559921Methyl (3,5-difluorophenyl)[1-(diphenylmethyl)azetidin-3-ylidene]acetate

생성물 1

HCID 67065947Methyl azetidin-3-yl(3,5-difluorophenyl)acetate

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 313Hydrochloric Acid용매HCID 887Methanol용매HCID 3283Diethyl Ether용매

실험 절차

A mixture of 0.406 g (1 mmol) of methyl (3,5-difluorophenyl)[1-(diphenylmethyl)azetidin-3-ylidene]acetate and 25 mg of 10% Pd/C in 10 mL of methanol and 1 mL of 1M HCl in ether was shaken under 40 psi H2 for 18 h. The mixture was filtered through CELITE and the solid residue was washed with 30 mL of methanol. The filtrate was concentrated to afford a mixture of the title compound and diphenylmethane, which was not separated but was used directly in the next step; Mass Spectrum: m/e=242 (M+1).

후처리

  1. filtrationThe mixture was filtered through CELITE
  2. washthe solid residue was washed with 30 mL of methanol
  3. concentrationThe filtrate was concentrated
  4. customto afford

출처 및 근거

ORD 기록
ord-22b7301a0a3643f9ba0f82d498f46810
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07485732B2

반응 노트

불러오는 중…