Phosphorus oxychloride → 3-(p-Bromophenyl)-6-chloro-4-methylpyridazine

HRID 372707노트

반응식

HRID 372707 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([CH3:15])=[CH:10][C:11](=O)[NH:12][N:13]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([Cl:18])=[CH:10][C:9]=2[CH3:15])=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychloride2회HCID 233336686-(p-bromophenyl)-5-methyl-3(2H)-pyridazinone

생성물 1

HCID 203982893-(p-Bromophenyl)-6-chloro-4-methylpyridazine

실험 절차

A 2.0 g. portion of 6-(p-bromophenyl)-5-methyl-3(2H)-pyridazinone and 20 ml. of phosphorus oxychloride are heated on a steam bath for 3 hours. The reaction mixture is poured slowly into crushed ice. The excess phosphorus oxychloride is decomposed. The solid which forms is recovered by filtration, washed with water, dried and recrystallized twice from chloroform, yielding 6-(p-bromophenyl)-5-methyl-3-chloropyridazine, m.p. 197°-200° C.

후처리

  1. additionThe reaction mixture is poured slowly
  2. custominto crushed ice
  3. filtrationThe solid which forms is recovered by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized twice from chloroform

출처 및 근거

ORD 기록
ord-7e7c0c4026c44048b47fb1c593e43e72
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04092311

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