反応 #1350588

ord-06b0b366a69140308df118a7f6eb5f76

反応方程式

C1COCCOCCOCCOCCO1
15-crown-5
O=S(=O)(O)O
sulfuric acid
COC(=O)c1cccc(N)c1C
methyl 3-amino-2-methylbenzoate
N#C[S-].[Na+]
sodium thiocyanate
COC(=O)c1cccc(NC(N)=S)c1C
N-(2-Methyl-3-methoxycarbonylphenyl)thiourea

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling
  2. 2
    ろ過the solid was filtered off with.suction,
  3. 3
    洗浄washed with water
  4. 4
    その他dried

実験手順

90.7 g of methyl 3-amino-2-methylbenzoate (0.55 mol) were dissolved in 510 ml of chlorobenzene and, at −5° C., admixed with 14 ml of conc. sulfuric acid and 49 g of sodium thiocyanate (0.6 mol). 2 ml of 15-crown-5 were then added, and the reaction mixture was heated at 100° C. for 13 h. After cooling, the solid was filtered off with.suction, washed with water and dried. Yield: 104.8 g (85%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06541423B1uspto-grants-2003_04