反応 #2006480

ord-c1d71aaff6ff47f2981f1ae9a49ce1ce

反応方程式

CC1(C)NC(=O)N(c2ccc(C#N)c(C(F)(F)F)c2)C1=N
compound 10a
CC1(C)NC(=O)N(c2ccc(C#N)c(C(F)(F)F)c2)C1=N
4-(4,4-Dimethyl-5-imino-2-oxo-1-imidazolidinyl)-2-trifluoromethyl-benzonitrile
O=C([O-])O
bicarbonate
CC1(C)NC(=O)N(c2ccc(C#N)c(C(F)(F)F)c2)C1=O
desired compound 11a
収率 95.0%
CC1(C)NC(=O)N(c2ccc(C#N)c(C(F)(F)F)c2)C1=O
4-(4,4-Dimethyl-2,5-dioxo-1-imidazolidinyl)-2-trifluoromethyl-benzonitrile
収率 95.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 35 min
  2. 2
    抽出extracted
  3. 3
    洗浄The organic layer was washed with brine
  4. 4
    乾燥finally dried over magnesium sulphate

実験手順

A suspension of the compound 10a in 6N HCl (25 mL) was refluxed for 35 min. The cooled solution was poured in a 10% bicarbonate solution, extracted using ethyl acetate (3×25 mL). The organic layer was washed with brine, and finally dried over magnesium sulphate to give of desired compound 11a (950 mg, 95%) which was used as such in the next step. 1H NMR (300 MHz, Acetone-d6) δ: 1.54 (s, 6H), 7.81 (broad s, 1H), 8.17 (m, 2H), 8.26 (s, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08168627B2uspto-grants-2012_05