HCID 21106512, compound → HCID 21106487, compound
Reaction equation
C(OC([N:8]([C:26]1[CH:30]=[C:29]([CH3:31])[N:28](C(OC(C)(C)C)=O)[N:27]=1)[C:9]1[C:18]2[C:13](=[CH:14][C:15]([C:19]([OH:21])=[O:20])=[CH:16][CH:17]=2)[C:12](=[O:22])[N:11]([CH:23]([CH3:25])[CH3:24])[N:10]=1)=O)(C)(C)C>C(O)(C(F)(F)F)=O.C(Cl)Cl>[CH:23]([N:11]1[C:12](=[O:22])[C:13]2[C:18](=[CH:17][CH:16]=[C:15]([C:19]([OH:21])=[O:20])[CH:14]=2)[C:9]([NH:8][C:26]2[CH:30]=[C:29]([CH3:31])[NH:28][N:27]=2)=[N:10]1)([CH3:25])[CH3:24]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
1-[tert-Butoxycarbonyl-(1-tert-butoxycarbonyl-5-methyl-1H-pyrazol-3-yl)-amino]-3-isopropyl-4-oxo-3,4-dihydro-phthalazine-6-carboxylic acid (13.0 mg, 0.02 mmol) was dissolved in a 20% TFA/DCM solution (2 ml) and the reaction mixture was stirred for 48 hours. After this time, the reaction mixture was concentrated and the resulting residue was triturated with diethyl ether to give the title compound (Example M-1) as a white solid. 1H-NMR: (400 MHz, D6- DMSO), 9.34(1H, s), 8.73 (1H, s), 8.47 (1H, d), 8.26 (1H, d), 6.28 (1H, s), 5.20-5.17 (1H, m), 2.19 (3H, s), 1.26 (6H, d) MS (ESI+)=(M+H)+ 328.31.
Workup
- concentrationAfter this time, the reaction mixture was concentrated
- customthe resulting residue was triturated with diethyl ether
Sources & evidence
- ORD record
- ord-d2a1829b0ff74d888e124005d86356a3
- Source dataset
- uspto-grants-2009_03
- Patent number
- US07501410B2
Reaction notes
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