Reaction equation
C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.[CH2:15]1[NH:20][CH2:19][CH2:18][N:17]2[CH2:21][CH2:22][CH2:23][CH2:24][C@H:16]12.C(N(C(C)C)CC)(C)C.Cl[C:35]1[N:36]=[N:37][C:38]([C:41]2[CH:46]=[CH:45][C:44]([C:47]([F:50])([F:49])[F:48])=[CH:43][CH:42]=2)=[CH:39][CH:40]=1>ClCCl.CS(C)=O>[F:50][C:47]([F:48])([F:49])[C:44]1[CH:43]=[CH:42][C:41]([C:38]2[N:37]=[N:36][C:35]([N:20]3[CH2:19][CH2:18][N:17]4[CH2:21][CH2:22][CH2:23][CH2:24][C@@H:16]4[CH2:15]3)=[CH:40][CH:39]=2)=[CH:46][CH:45]=1Participants
7
Reactant 4
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 160 °C
Procedure
A mixture of the dihydrochloride salt of (R)-octahydropyrido[1,2-a]pyrazine (649 mg, 3.05 mmol), diisopropylethylamine (1.17 ml, 6.72 mmol), 3-chloro-6-(4-trifluoromethylphenyl)-pyridazine (290 mg, 1.12 mmol) and dimethylsulfoxide (1 ml) was heated in a closed vessel at 160° C. for 40 min. The reaction mixture was cooled to room temperature, diluted with dichloromethane (10 ml) and washed with water (2×15 ml) and brine (15 ml). The organic layer was dried over magnesium sulphate. The solvent was removed in vacuo to give 398 mg of the title compound as the free base.
Workup
- temperatureThe reaction mixture was cooled to room temperature
- washwashed with water (2×15 ml) and brine (15 ml)
- dry with materialThe organic layer was dried over magnesium sulphate
- customThe solvent was removed in vacuo
Sources & evidence
- ORD record
- ord-bfd189a0842d47fd8b77df7eb5d727b1
- Source dataset
- uspto-grants-2007_03
- Patent number
- US07186721B2
Linked notes
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