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Acetic Acid → HCID 136389259, compound

HRID 1517394
Notes
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Reaction equation

HRID 1517394 reaction equation
[NH2:1][C:2]1[NH:3][C:4](=[O:22])[C:5]2[N:11]=[C:10]([C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[C:14]([O:20][CH3:21])[CH:13]=3)[CH:9]=[CH:8][C:6]=2[N:7]=1.[C:23](O)(=[O:25])[CH3:24]>C(OC(=O)C)(=O)C>[C:23]([NH:1][C:2]1[NH:3][C:4](=[O:22])[C:5]2[N:11]=[C:10]([C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[C:14]([O:20][CH3:21])[CH:13]=3)[CH:9]=[CH:8][C:6]=2[N:7]=1)(=[O:25])[CH3:24]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 1362700182-Amino-6-(3,4-dimethoxyphenyl)pyrido[3,2-d]pyrimidin-4(1H)-one

Product 1

HCID 136389259HCID 136389259, compoundYield 77%

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

2-amino-6-(3,4-dimethoxyphenyl)-pyrido[3,2-d]pyrimidin-4(3H)-one (2.0 g, 6.70 mmol) was suspended in acetic anhydride (180 ml) and acetic acid (20 ml) and the mixture was refluxed for 16 hours. The hot suspension was filtered and the filtrate was concentrated under reduced pressure until crystallization started. The precipitate was filtered off to give the pure title compound (1.76 g, yield 77%) which was characterized by its mass spectrum as follows: MS (m/z): 341 ([M+H]+, 100).

Workup

  1. filtrationThe hot suspension was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure until crystallization
  3. filtrationThe precipitate was filtered off

Sources & evidence

ORD record
ord-02c12462fd6440788eed3d0c757f861e
Source dataset
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08232278B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes