Hydrogen chloride-ethyl acetate → HCID 178492353, compound
Reaction equation
C(OC([NH:8][C:9]([NH:18][C@@H:19]1[CH2:24][CH2:23][CH2:22][CH2:21][C@@H:20]1[NH:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[C:33]([CH3:36])[CH:34]=2)[N:29]=[C:28]([C:37]([NH:39][C:40]2[CH:45]=[CH:44][C:43]([O:46][CH3:47])=[CH:42][CH:41]=2)=[O:38])[N:27]=1)=[N:10]C(OC(C)(C)C)=O)=O)(C)(C)C.C(OCC)(=O)C.[ClH:54]>CO.C(Cl)(Cl)Cl>[ClH:54].[ClH:54].[NH2:10][C:9]([NH:18][C@@H:19]1[CH2:24][CH2:23][CH2:22][CH2:21][C@@H:20]1[NH:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[C:33]([CH3:36])[CH:34]=2)[N:29]=[C:28]([C:37]([NH:39][C:40]2[CH:41]=[CH:42][C:43]([O:46][CH3:47])=[CH:44][CH:45]=2)=[O:38])[N:27]=1)=[NH:8]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
To a solution of 2.07 g of 4-{[(1S,2R)-2-({(tert-butoxycarbonyl)amino[(tert-butoxycarbonyl)imino]methyl}amino)cyclohexyl]amino}-N-(4-methoxyphenyl)-6-methylquinazoline-2-carboxamide in 10 ml of methanol and 10 ml of chloroform, 40 ml of a 4N-hydrogen chloride-ethyl acetate solution was added, and then the mixture was reacted at 50° C. for 15 hours. The reaction solution was concentrated and recrystallized from methanol-diisopropyl ether to obtain 952 mg of the desirable compound as a yellow powder.
Workup
- customthe mixture was reacted at 50° C. for 15 hours
- concentrationThe reaction solution was concentrated
- customrecrystallized from methanol-diisopropyl ether
Sources & evidence
- ORD record
- ord-e48dc153477b4886bc23d4534476ce48
- Source dataset
- uspto-grants-2010_05
- Patent number
- US07718663B2
Reaction notes
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