1,4-Dioxane hydrochloride → HCID 69203803, compound
Reaction equation
[F:1][C:2]([F:28])([F:27])[C:3]1[N:26]=[CH:25][C:6]2[CH2:7][N:8](C(OC(C)(C)C)=O)[N:9](C(OC(C)(C)C)=O)[CH2:10][C:5]=2[CH:4]=1.[ClH:29].O1CCOCC1>>[ClH:29].[F:27][C:2]([F:1])([F:28])[C:3]1[N:26]=[CH:25][C:6]2[CH2:7][NH:8][NH:9][CH2:10][C:5]=2[CH:4]=1Participants
3
Procedure
A solution of the product from Step C (4.53 g, 11.24 mmol) in 4N HCl/Dioxane (55 ML, 225 mmol) was stirred overnight. The solvent was evaporated to yield the 7-(trifluoromethyl)-1,2,3,4-tetrahydropyrido[3,4-d]pyridazine HCl salt (2.98 g, 100%). 1H-NMR (400 MHz, CD3OD) δ 8.63 (s, 1H), 7.78 (s, 1H), 4.80 (s, 2H), 4.48 (s, 2H). ESI-MS calc. For C8H8F3N3: 203.07; Found: 204 (M+H).
Workup
- customThe solvent was evaporated
Sources & evidence
- ORD record
- ord-f357a1256ddc466287914b1ed68eb87e
- Source dataset
- uspto-grants-2008_07
- Patent number
- US07393844B2
Reaction notes
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