5-(4-benzyloxy-phenyl)-6-trifluoromethyl-2H-pyridazin-3-one → 4-(4-Benzyloxy-phenyl)-6-chloro-3-trifluoromethyl-pyridazine

HRID 401890노트

반응식

HRID 401890 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:20]([C:21]([F:24])([F:23])[F:22])=[N:19][NH:18][C:17](=O)[CH:16]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O(Cl)[Cl:27].[P+5]>>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[C:17]([Cl:27])[N:18]=[N:19][C:20]=2[C:21]([F:24])([F:23])[F:22])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 673755765-(4-benzyloxy-phenyl)-6-trifluoromethyl-2H-pyridazin-3-oneHCID 178479711HCID 178479711, 화합물

생성물 1

HCID 866577774-(4-Benzyloxy-phenyl)-6-chloro-3-trifluoromethyl-pyridazine

반응 조건

온도
90 °C

실험 절차

A mixture of the 5-(4-benzyloxy-phenyl)-6-trifluoromethyl-2H-pyridazin-3-one (0.491 mmol, 170 mg) and phosphorus(V) oxychloride may be heated at 90° C. for 2 h. The reaction mixture may be concentrated in vacuo, and ice may be added to the residue. The mixture may be neutralized with solid sodium bicarbonate and extracted with diethyl ether. Purification by column chromatography on silica gel gives 4-(4-benzyloxy-phenyl)-6-chloro-3-trifluoromethyl-pyridazine as a white solid.

후처리

  1. concentrationThe reaction mixture may be concentrated in vacuo, and ice
  2. additionmay be added to the residue
  3. extractionextracted with diethyl ether
  4. customPurification by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-7e5c46193d9f4e9691952ff1b15153ec
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741900B2

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