Phosphorus oxychloride → 3-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

HRID 372730ノート

反応式

HRID 372730 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[CH:10]=[CH:11][C:12](=O)[NH:13][N:14]=2)[CH:4]=1.P(Cl)(Cl)([Cl:20])=O>>[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]=[N:13][C:12]([Cl:20])=[CH:11][CH:10]=2)[CH:4]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 124495416-[3-(Trifluoromethyl)phenyl]pyridazin-3-ol

生成物 1

HCID 124495523-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

実験手順

A mixture of 12.6 g. of 6-(α,α,α-trifluoro-m-tolyl)-3(2H)-pyridazinone and 200 ml. of phosphorus oxychloride is heated on a steam bath for 18 hours. The mixture is concentrated under vacuum and the residue triturated with cold water. The resulting solid is washed with water and air dried to give 13.5 g. of cream colored crystals, m.p. 131°-133° C. Recrystallization from methanol gives 6-(α,α,α-trifluoro-m-tolyl)-3-chloropyridazine as white crystals, m.p. 131°-133° C.

後処理

  1. additionA mixture of 12.6 g
  2. concentrationThe mixture is concentrated under vacuum
  3. customthe residue triturated with cold water
  4. washThe resulting solid is washed with water and air
  5. customdried
  6. customto give 13.5 g
  7. customRecrystallization from methanol

出典と根拠

ORDレコード
ord-de7977de5bee49989108fd2055ef3762
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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