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Ammonia → HCID 178513810, 화합물

HRID 392371
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HRID 392371 반응식
[F:1][C:2]1[N:7]=[C:6]([C:8](OC)=[O:9])[C:5](=[O:12])[NH:4][CH:3]=1.[NH3:13].C(OCC)(=O)C.C(=O)([O-])O.[Na+]>CO.O>[F:1][C:2]1[N:7]=[C:6]([C:8]([NH2:13])=[O:9])[C:5]([OH:12])=[N:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 22662805HCID 22662805, 화합물

생성물 1

HCID 178513810HCID 178513810, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water
용매

실험 절차

In 3.0 mL of methanol was dissolved 0.12 g of methyl 6-fluoro-3-oxo-3,4-dihydro-2-pyrazinecarboxylate. Then, gaseous ammonia was introduced into the solution at an ice-cooled temperature for a period of 10 minutes, after which the mixture thus obtained was allowed to stand at room temperature for 2 days. The solvent was removed under reduced pressure, the residue thus obtained was added to a mixture of 30 mL of ethyl acetate and 30 ml of water, pH was adjusted to 7.5 with saturated aqueous solution of sodium hydrogen carbonate, and the organic layer was separated. After adding 30 mL of ethyl acetate to the remaining aqueous layer, pH was adjusted to 1.0 with 1 mol/L hydrochloric acid, and the whole mixture was extracted with two 15 mL portions of ethyl acetate. The organic layers thus obtained were united, washed successively with 15 mL of water and 15 mL of saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The solid product thus obtained was washed with diisopropyl ether to obtain 0.015 g of 6-fluoro-3-hydroxy-2-pyrazinecarboxamide as a yellow-colored solid product.

후처리

  1. temperaturecooled temperature for a period of 10 minutes
  2. customafter which the mixture thus obtained
  3. customThe solvent was removed under reduced pressure
  4. customthe residue thus obtained
  5. customthe organic layer was separated
  6. additionAfter adding 30 mL of ethyl acetate to the remaining aqueous layer, pH
  7. extractionthe whole mixture was extracted with two 15 mL portions of ethyl acetate
  8. customThe organic layers thus obtained
  9. washwashed successively with 15 mL of water and 15 mL of saturated aqueous solution of sodium chloride
  10. dry with materialdried on anhydrous magnesium sulfate
  11. customthe solvent was removed under reduced pressure
  12. customThe solid product thus obtained
  13. washwas washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-3b8eb7ff3c6d447cb1bde78e50816186
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06800629B2

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