Réaction #2358493

ord-c985030f22484b65a5990c8fd3b0d2bc

Équation de réaction

[Cl-].[Cl-].[Mg+2]
magnesium chloride
CC1=CC(O/C=C2/C(=O)N(C(=O)OC(C)(C)C)C3C=CCC23)OC1=O
tert-butyl (3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]-2-oxo-4,6a-dihydro-3aH-cyclopenta[b]pyrrole-1-carboxylate
ClCCl
CH2Cl2
CC1=CC(O/C=C2/C(=O)NC3C=CCC23)OC1=O
desired compound
Rendement 40.0%
CC1=CC(O/C=C2/C(=O)NC3C=CCC23)OC1=O
(3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]-1,3a,4,6a-tetrahydrocyclopenta[b]pyrrol-2-one
Rendement 40.0%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Filtrationfiltrated
  2. 2
    Concentrationconcentrated
  3. 3
    Autrepurified by flash chromatography (EtOAc

Mode opératoire

A solution of tert-butyl (3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]-2-oxo-4,6a-dihydro-3aH-cyclopenta[b]pyrrole-1-carboxylate Ib-1 (28 mg, 0.080 mmol) in acetonitrile (1 mL) was stirred with magnesium chloride (23 mg, 0.24 mmol) at 40° C. for 7 h. The solution was then diluted into CH2Cl2, filtrated, concentrated and purified by flash chromatography (EtOAc, then 5% MeOH in CH2Cl2) giving the desired compound as a colorless oil (8 mg, 40%); 1H NMR (400 MHz, CDCl3) 7.27 (1H, s), 6.93 (1H, s), 6.54 (1H, brs), 6.14 (1H, s), 5.87 (1H, d), 5.71 (1H, brs), 4.65 (1H, d), 3.66 (1H, m), 2.83 (1H, m), 2.46 (1H, d), 2.02 (3H, s): LCMS (Method A): 0.63 min; ES+270 (M+Na+).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09119398B2uspto-grants-2015_09