反応 #220424

ord-d12a28f6b36f4d40a09ee120657699ed

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling to 23° C. the mixture
  2. 2
    洗浄washed with several portions of brine
  3. 3
    乾燥dried over Na2SO4
  4. 4
    その他The title compound was purified by chromatography (SiO2, CHCl3/MeOH 9:1)

実験手順

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (0.2 g, 0.617 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (0.22 g, 0.678 mmol) and warmed to 60° C. To the reaction mixture was added 1-iodo-2-methylpropane (0.078 ml, 0.678 mmol) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3/MeOH 9:1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07390801B2uspto-grants-2008_06