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

반응식

HRID 517818 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-24d36e55a3634928a611084a77e601cb
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115134B2

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