Phosphorus oxychloride → 4-chloro-1-(4-chlorobenzyl)-1,3,5-triazin-2(1H)-one

HRID 1477573ノート

反応式

HRID 1477573 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]2[CH:12]=[N:11][C:10](O)=[N:9][C:8]2=[O:14])=[CH:4][CH:3]=1.C(N(CC)C(C)C)(C)C.P(Cl)(Cl)([Cl:28])=O>C1(C)C=CC=CC=1>[Cl:28][C:10]1[N:11]=[CH:12][N:7]([CH2:6][C:5]2[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:8](=[O:14])[N:9]=1

参加物

5

反応物 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 178518532HCID 178518532、化合物

生成物 1

HCID 1178396204-chloro-1-(4-chlorobenzyl)-1,3,5-triazin-2(1H)-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

A toluene solution (25 mL) of 1-(4-chlorobenzyl)-4-hydroxy-1,3,5-triazin-2(1H)-one (600 mg, 2.52 mmol) synthesized in Reference Synthesis Example 10, N,N-diisopropylethylamine (0.52 mL, 4.63 mmol), and phosphorus oxychloride (0.94 mL) was stirred at 70° C. for 30 minutes. After completion of the reaction, the reaction solution was concentrated under reduced pressure and toluene was added, followed by concentrating the resultant mixture under reduced pressure again. To the obtained crude product of 4-chloro-1-(4-chlorobenzyl)-1,3,5-triazin-2(1H)-one, chloroform was added and the resultant solution was used in the next reaction as the chloroform solution.

後処理

  1. customAfter completion of the reaction
  2. concentrationthe reaction solution was concentrated under reduced pressure and toluene
  3. additionwas added
  4. concentrationby concentrating the resultant mixture under reduced pressure again

出典と根拠

ORDレコード
ord-50e59b5182ff4783af6480e496d8f6e3
出典データセット
uspto-grants-2016_08
特許番号
US09403798B2

反応ノート

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