3-Chloro-6-(4-fluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazine → 3-Chloro-6-(4-fluorophenyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine

HRID 517818

反応式

HRID 517818 の反応式
[Cl:1][C:2]1[N:6]2[N:7]=[C:8]([C:11]3[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=3)[CH:9]=[CH:10][C:5]2=[N:4][N:3]=1>C(O)(=O)C.[Zn]>[Cl:1][C:2]1[N:6]2[N:7]=[C:8]([C:11]3[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=3)[CH2:9][CH2:10][C:5]2=[N:4][N:3]=1

参加物

4

反応物 1

HCID 446043783-Chloro-6-(4-fluorophenyl)-[1,2,4]triazolo[4,3-b]pyridazine

生成物 1

HCID 675246973-Chloro-6-(4-fluorophenyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine収率 87%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

790 mg of zinc powder are added to a mixture of 300 mg of 3-chloro-6-(4-fluorophenyl)[1,2,4]triazolo[4,3-b]pyridazine in 10 cm3 of glacial acetic acid at 20° C. After stirring for 1 h, the suspension is filtered and the filtrate is concentrated to dryness under vacuum. The oily residue is purified by dry deposit on Biotage Quad 12M (KP-SIL, 60 Å; 32-63 μm), elution being carried out with a 95:5 mixture of dichloromethane/methanol. 263 mg of 3-chloro-6-(4-fluorophenyl)-7,8-dihydro[1,2,4]triazolo[4,3-b]pyridazine are thus obtained in the form of a yellowy-brown powder, the characteristics of which are as follows:

後処理

  1. filtrationthe suspension is filtered
  2. concentrationthe filtrate is concentrated to dryness under vacuum
  3. customThe oily residue is purified
  4. customby dry deposit
  5. washon Biotage Quad 12M (KP-SIL, 60 Å; 32-63 μm), elution
  6. additionbeing carried out with a 95:5 mixture of dichloromethane/methanol

出典と根拠

ORDレコード
ord-24d36e55a3634928a611084a77e601cb
出典データセット
uspto-grants-2015_08
特許番号
US09115134B2

関連ノート

読み込み中…