Ammonia → Pyridine, 2,3,5-trichloro-

HRID 1577302ノート

反応式

HRID 1577302 の反応式
[Cl:1][C:2]1[C:3](=O)[NH:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.CN(C)C=O.C(Cl)([Cl:17])=O.N>C1(C)C=CC=CC=1.O>[Cl:17][C:3]1[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][N:4]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 6371Phosgene3 回HCID 794963,5-Dichloro-2-pyridone3 回

生成物 1

HCID 27666Pyridine, 2,3,5-trichloro-

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

According to a preferred embodiment of the process of the invention, 3,5-dichloro-2-pyridone is suspended in toluene, the water present is separated by azeotropic distillation, 0.05-0.15 mol of N,N-dimethylformamide per mol of 3,5-dichloro-2-pyridone is added, and 1.0-1.3 mols of phosgene per mol of 3,5-dichloro-2-pyridone are introduced at 75°-80° C. After the addition of phosgene has been completed, the reaction mixture is allowed to react for a further one hour at 75°-80° C., and the excess phosgene is subsequently reacted with aqueous ammonia. The phases are afterwards separated, the solvent is distilled off from the organic phase, and 2,3,5-trichloropyridine is obtained as a melt.

後処理

  1. additionis added
  2. customto react for a further one hour at 75°-80° C.
  3. customThe phases are afterwards separated
  4. distillationthe solvent is distilled off from the organic phase

出典と根拠

ORDレコード
ord-85ae844b97d348faa666c72975d337ed
出典データセット
uspto-grants-1981_09
特許番号
US04287347

反応ノート

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