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HCID 10339510, compound → HCID 10607909, compound

HRID 1289762
Notes
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Reaction equation

HRID 1289762 reaction equation
NC1N=[C:5]([C:7]2C=[C:11](C(C)(C)C)[C:10](OCOCCOC)=[C:9](C(C)(C)C)[CH:8]=2)[NH:4]N=1.C[O-].[Na+].CO.[C:33]([NH:36][NH2:37])([NH2:35])=[NH:34].[ClH:38]>CO>[NH2:34][C:33]1[N:35]=[C:11]([C:10]2[CH:9]=[CH:8][C:7]([Cl:38])=[CH:5][N:4]=2)[NH:37][N:36]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 10339510HCID 10339510, compoundHCID 23694274Sodium methanolate methanolHCID 178418668HCID 178418668, compound

Product 1

HCID 10607909HCID 10607909, compoundYield 82%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The synthesis method of Example 7-(2) was applied. The compound (3.94 g) obtained in (3) above, a 5M sodium methoxide-methanol solution (17 ml), methanol (20 ml) and aminoguanidine hydrochloride (9.39 g) were used as reagents. The mixture was stirred with refluxing for 18 hours and methanol was distilled away under reduced pressure. Water was added to the residue and the aqueous layer was adjusted to pH 3-4 with 3N hydrochloric acid to give 3.40 g of a pale-yellow solid that precipitated (yield 82%).

Workup

  1. temperaturewith refluxing for 18 hours
  2. distillationmethanol was distilled away under reduced pressure
  3. additionWater was added to the residue

Sources & evidence

ORD record
ord-611c5913e9194cf5b626e48d685ad9c3
Source dataset
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05750545

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes