반응 #1869186

ord-8d9dc825fe334515b6fc7488d845bd7e

반응 방정식

N#Cc1ccc(N)cc1
4-amino-benzonitrile
CC1(C)OC(=O)CC(=O)O1
2,2-dimethyl-[1,3]dioxane-4,6-dione
COC(OC)OC
trimethylorthoformate
CC1(C)OC(=O)C(=CNc2ccc(C#N)cc2)C(=O)O1
solid
수율 97.0%
CC1(C)OC(=O)C(=CNc2ccc(C#N)cc2)C(=O)O1
4-[(2,2-Dimethyl-4,6-dioxo-[1,3]dioxan-5-ylidenemethyl)-amino]-benzonitrile
수율 97.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 3 hours
  2. 2
    온도After cooling the solid
  3. 3
    여과was filtered off
  4. 4
    세척washed with ethanol and air
  5. 5
    기타dried

실험 절차

A mixture of 4-amino-benzonitrile (12.5 g, 0.106 mol), 2,2-dimethyl-[1,3]dioxane-4,6-dione (18.3 g, 0.127 mol) and trimethylorthoformate (16 ml) in ethanol (100 ml) was refluxed for 3 hours. After cooling the solid was filtered off, washed with ethanol and air dried. The product was obtained as an off-white solid (27.9 g, 97%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07498326B2uspto-grants-2009_03