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

HRID 1971896ノート

反応式

HRID 1971896 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-db2fce6c176d4a1d87d22cdb9abd5276
出典データセット
uspto-grants-2013_04
特許番号
US08431575B2

反応ノート

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