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Carbonic acid-guanidine (1:1) → HCID 178433373, compound

HRID 2387840
Notes
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Reaction equation

HRID 2387840 reaction equation
O=[C:2]([CH3:24])[CH:3]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][O:17][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][O:19]2)=[CH:12][CH:11]=1)[C:4](OCC)=[O:5].C(=O)(O)O.[NH2:29][C:30]([NH2:32])=[NH:31]>CCO>[NH2:32][C:30]1[N:31]=[C:4]([OH:5])[C:3]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][O:17][CH:18]3[CH2:23][CH2:22][CH2:21][CH2:20][O:19]3)=[CH:12][CH:11]=2)=[C:2]([CH3:24])[N:29]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 286947Carbonic acid-guanidine (1:1)HCID 68414491Ethyl 3-oxo-2-(4-((tetrahydro-2H-pyran-2-yloxy)methyl)benzyl)butanoate

Product 1

HCID 178433373HCID 178433373, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of the product from step (i) (15.66 g) and guanidine carbonate (8.7 g) in EtOH (150 ml) was heated under reflux for 48 h. The mixture was cooled, the solvent removed under reduced pressure and the residue triturated with water. The solid was filtered, washed with water then diethylether and dried to afford the subtitle compound, 11.58 g.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 48 h
  3. temperatureThe mixture was cooled
  4. customthe solvent removed under reduced pressure
  5. customthe residue triturated with water
  6. filtrationThe solid was filtered
  7. washwashed with water
  8. dry with materialdiethylether and dried

Sources & evidence

ORD record
ord-59091e8e39674a8595ecc191d4a19b2f
Source dataset
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08268990B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes