反応 #4252

ord-41d0738c14934a8d8d2f0c0151409174

反応方程式

CCOC(=O)c1ccc(N)cc1
ethyl p-aminobenzoate
Clc1nc(Cl)nc(Cl)n1
cyanuric chloride
Cl
hydrogen chloride
CCOC(=O)c1ccc(NN2CN(Nc3ccc(C(=O)OCC)cc3)CN(Nc3ccc(C(=O)OCC)cc3)C2)cc1
1,3,5-tris-(p-ethoxycarbonylanilino)-s-triazine
収率 97.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄the suspension, at 80°-90° C., was washed neutral with saturated sodium bicarbonate solution
  2. 2
    ろ過the product was filtered off over a glass suction
  3. 3
    ろ過filter
  4. 4
    その他The white crystals obtained
  5. 5
    洗浄were washed with ethanol
  6. 6
    その他dried

実験手順

82.6 g of ethyl p-aminobenzoate and 30.75 g of cyanuric chloride in 1,500 ml of xylene were refluxed for 8 hours, hydrogen chloride escaping during this procedure. Thereafter, 1 liter of xylene was added, and the suspension, at 80°-90° C., was washed neutral with saturated sodium bicarbonate solution and then cooled to room temperature, and the product was filtered off over a glass suction filter. The white crystals obtained were washed with ethanol and dried. Mp: 218°-223° C.; yield: 97% of 1,3,5-tris-(p-ethoxycarbonylanilino)-s-triazine; ultraviolet (in ethanol): E1 cm1% =2,080 at 313 nm, E1 cm1% =699 at 218 nm.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04724137uspto-grants-1988_02