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

HRID 372707ノート

反応式

HRID 372707 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychloride2 回HCID 233336686-(p-bromophenyl)-5-methyl-3(2H)-pyridazinone

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7e7c0c4026c44048b47fb1c593e43e72
出典データセット
uspto-grants-1978_05
特許番号
US04092311

反応ノート

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