Hydrochloric Acid → HCID 68516930, compound

HRID 1513095Notes

Reaction equation

HRID 1513095 reaction equation
C(OC([NH:8][CH2:9][C:10]1[N:18]=[C:17]2[C:13]([NH:14][C:15](=[O:40])[N:16]2[C:19]2[CH:24]=[C:23]([O:25][CH2:26][C:27]3[C:32]([O:33][CH3:34])=[CH:31][CH:30]=[C:29]([F:35])[C:28]=3[F:36])[C:22]([O:37][CH3:38])=[CH:21][C:20]=2[Cl:39])=[C:12]([O:41][CH3:42])[N:11]=1)=O)(C)(C)C.Cl.C(OCC)C>O1CCCC1>[ClH:39].[NH2:8][CH2:9][C:10]1[N:18]=[C:17]2[C:13]([NH:14][C:15](=[O:40])[N:16]2[C:19]2[CH:24]=[C:23]([O:25][CH2:26][C:27]3[C:32]([O:33][CH3:34])=[CH:31][CH:30]=[C:29]([F:35])[C:28]=3[F:36])[C:22]([O:37][CH3:38])=[CH:21][C:20]=2[Cl:39])=[C:12]([O:41][CH3:42])[N:11]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 59309896HCID 59309896, compound

Product 1

HCID 68516930HCID 68516930, compoundYield 86.9%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 2-(tert-butoxycarbonylaminomethyl)-9-[2-chloro-5-(2,3-difluoro-6-methoxybenzyloxy)-4-methoxyphenyl]-6-methoxy-7,9-dihydro-8H-purin-8-one (36 mg) in tetrahydrofuran (1 mL) was added hydrochloric acid (4 mol/L ethyl acetate solution, 2 mL) under ice-cooling, and the mixture was stirred at the same temperature for 1 hour, and then stirred at room temperature for 3 hours. To the reaction mixture was added diethyl ether, and the insoluble material was collected by filtration. The collected material was washed with diethyl ether, and dried under reduced pressure to give the title compound (14 mg).

Workup

  1. temperaturecooling
  2. stirringstirred at room temperature for 3 hours
  3. filtrationthe insoluble material was collected by filtration
  4. washThe collected material was washed with diethyl ether
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-2e924351643a4d909c06a3e3f00c38ed
Source dataset
uspto-grants-2012_07
Patent number
US08217069B2

Reaction notes

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