Water → 8-(6-Chloropyridazin-3-yl)-1,4-dioxa-8-azaspiro[4.5]decane
Reaction equation
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][CH:7]=1.[O:9]1[C:13]2([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[O:12][CH2:11][CH2:10]1.CCN(C(C)C)C(C)C.O>CS(C)=O>[Cl:1][C:2]1[N:3]=[N:4][C:5]([N:16]2[CH2:17][CH2:18][C:13]3([O:12][CH2:11][CH2:10][O:9]3)[CH2:14][CH2:15]2)=[CH:6][CH:7]=1Participants
6
Conditions
- Temperature
- 80 °C
Procedure
To a mixture of 3,6-dichloropyridazine (2.98 g, 20 mmol) in DMSO (10 mL) was added 1,4-dioxa-8-azaspiro[4.5]decane (3 g, 21 mmol) and DIPEA (4.18 mL, 24 mmol). The resulting mixture was heated at 80° C. for 4 h and was then poured into H2O (300 mL). The resulting solid was washed with H2O (10 mL×3) and hexane (10 mL×3) and then dried to yield 8-(6-chloropyridazin-3-yl)-1,4-dioxa-8-azaspiro[4.5]decane.
Workup
- washThe resulting solid was washed with H2O (10 mL×3) and hexane (10 mL×3)
- customdried
Sources & evidence
- ORD record
- ord-48dd55e183604a29bef038d5fe96d56f
- Source dataset
- uspto-grants-2015_08
- Patent number
- US09102669B2
Reaction notes
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