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

HRID 401890ノート

反応式

HRID 401890 の反応式
[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

参加物

3

反応物 2

HCID 673755765-(4-benzyloxy-phenyl)-6-trifluoromethyl-2H-pyridazin-3-oneHCID 178479711HCID 178479711、化合物

生成物 1

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

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7e5c46193d9f4e9691952ff1b15153ec
出典データセット
uspto-grants-2014_06
特許番号
US08741900B2

反応ノート

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