反応 #328730

ord-4febb7ba25a44d73a2ff288fa50b85b8

反応方程式

CC(C)(C)OC(=O)N1CCC(=O)C1
1-(tert-butoxylcarbonyl)-3-pyrrolidone
COC(OC)N(C)C
N,N-dimethylformamide dimethyl acetal
CN(C)C=C1CN(C(=O)OC(C)(C)C)CC1=O
tert-Butyl 3-[(dimethylamino)methylene]-4-oxopyrrolidine-1-carboxylate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was redissolved in a minimum amount of dichloromethane
  3. 3
    その他triturated with hexane
  4. 4
    その他to yield a yellow precipitate

実験手順

A solution of 1-(tert-butoxylcarbonyl)-3-pyrrolidone (4.10 g) and N,N-dimethylformamide dimethyl acetal (30.0 mL) was heated to 140° C. for 1 h. The resulting mixture was cooled to room temperature and concentrated under reduced pressure. The residue was redissolved in a minimum amount of dichloromethane and triturated with hexane to yield a yellow precipitate. LC-MS=241.1 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08653059B2uspto-grants-2014_02