Reaktion #312750

ord-9375a58ecd2242a4a6def5cdde1944ef

Reaktionsgleichung

CC(C)(C)OC(=O)N1CCC(=O)C1
N-BOC-3-pyrrolidone
COC(OC)N(C)C
N,N-dimethylformamide-dimethylacetal
CN(C)/C=C1/CN(C(=O)OC(C)(C)C)CC1=O
crude title compound
Ausbeute 90.0%
CN(C)/C=C1/CN(C(=O)OC(C)(C)C)CC1=O
3-[1-Dimethylamino-meth-(Z)-ylidene]-4-oxo-pyrrolidine-1-carboxylic acid tert.-butyl ester
Ausbeute 90.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was quenched by addition of 50 ml water
  2. 2
    Extraktionextracted 3 times with ethyl acetate
  3. 3
    TrocknenThe extract was dried over magnesium sulfate
  4. 4
    Einengenconcentrated

Vorschrift

A solution of 13.5 mmol N-BOC-3-pyrrolidone and 13.5 mmol N,N-dimethylformamide-dimethylacetal in 50 ml N,N-dimethylformamide was hold overnight at 60° C. The reaction mixture was quenched by addition of 50 ml water and extracted 3 times with ethyl acetate. The extract was dried over magnesium sulfate and concentrated to give the crude title compound as a yellowish oil. Yield=90%. MS (m/e): 241.4 ([M+H]+, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07557114B2uspto-grants-2009_07