反応 #73359

ord-fb4be5184a514e069f2c5ab7e30c45b6

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Reaction
  2. 2
    濃縮is concentrated in vacuo

実験手順

A mixture of 1-benzyl-2-methyl-3-oxo-piperidine-4-carboxylic acid methyl ester (1.0 g, 3.9 mmol), formamidine hydrochloride (930 mg, 11.6 mmol), and EtOH (6 mL) is treated with NaOEt solution (5.5 mL, 13.57 mmol, 21% w/w in EtOH) and the reaction is stirred at 90° C. for 2 h. Reaction is concentrated in vacuo after adjusting to pH 6. Residue is via semi-prep HPLC (C18; 10-100% I/H2O with 0.1% NH4OH) to give the title compound. MS (ESI) m/z 256.0 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541432B2uspto-grants-2013_09