反応 #302892

ord-ab661d7a8bcc4d6ba081a13baa6c3320

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    その他a solid precipitate that had formed
  3. 3
    ろ過was collected by filtration
  4. 4
    洗浄The solid was rinsed with diethyl ether
  5. 5
    その他was dried under reduced pressure

実験手順

Under a dry nitrogen atmosphere, a stirred mixture of 5.56 grams (0.041 mole) of 2,3-dimethylbenzylamine and 5.0 grams (0.041 mole) of 2-chloroethylisothiocyanate in 100 mL of 1,4-dioxane was heated to 80° C. where it stirred for about 18 hours. The reaction mixture was allowed to cool and a solid precipitate that had formed was collected by filtration. The solid was rinsed with diethyl ether and was dried under reduced pressure to yield 8.0 grams of the title compound. The NMR spectrum was consistent with the proposed structure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08193118B2uspto-grants-2012_06