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Calcium Carbonate → HCID 178513810, compound

HRID 392357
Notes
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Reaction equation

HRID 392357 reaction equation
[OH:1][C:2]1[C:3]([C:8]([NH2:10])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.[F:11]F.C(=O)([O-])[O-].[Ca+2]>O>[F:11][C:5]1[N:4]=[C:3]([C:8]([NH2:10])=[O:9])[C:2]([OH:1])=[N:7][CH:6]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 10112Calcium CarbonateHCID 24524Fluorine2×HCID 178513804HCID 178513804, compound

Product 1

HCID 178513810HCID 178513810, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In 200 mL of water was suspended 1.0 g of 3-hydroxy-2-pyrazinecarboxamide. At room temperature, 10% fluorine gas (a fluorine gas diluted with nitrogen gas) was introduced at a rate of 45 mL per minute for a period of 25 minutes. Then, nitrogen gas was introduced for 45 minutes, and the liquid reaction mixture was neutralized with calcium carbonate, the deposited precipitate was filtered off, the filtrate was concentrated under reduced pressure, and the solid product thus obtained was purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1] to obtain 0.008 g of 6-fluoro-3-hydroxy-2-pyrazinecarboxamide as a white-colored solid product.

Workup

  1. additionwas introduced at a rate of 45 mL per minute for a period of 25 minutes
  2. additionThen, nitrogen gas was introduced for 45 minutes
  3. customthe liquid reaction mixture
  4. filtrationthe deposited precipitate was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customthe solid product thus obtained
  7. customwas purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1]

Sources & evidence

ORD record
ord-db244f86290d46ee90463e77e2bc6cfb
Source dataset
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06800629B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes