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

HRID 1477573노트

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HRID 1477573 반응식
[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

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 178518532HCID 178518532, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50e59b5182ff4783af6480e496d8f6e3
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403798B2

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