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

HRID 372730

반응식

HRID 372730 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-de7977de5bee49989108fd2055ef3762
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04092311

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