Hydrochloric Acid → 4-(3,4-Difluorobenzyl)-3-oxo-3,4-dihydropyrazine-2-carboxylic acid

HRID 1038978노트

반응식

HRID 1038978 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[F:20])[CH2:5][N:6]1[CH:11]=[CH:10][N:9]=[C:8]([C:12]([O:14]C)=[O:13])[C:7]1=[O:16].[OH-].[Na+].Cl.[Cl-].[Na+]>C1COCC1>[F:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[F:20])[CH2:5][N:6]1[CH:11]=[CH:10][N:9]=[C:8]([C:12]([OH:14])=[O:13])[C:7]1=[O:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 58443085Methyl 4-(3,4-difluorobenzyl)-3-oxo-3,4-dihydropyrazine-2-carboxylate

생성물 1

HCID 584430534-(3,4-Difluorobenzyl)-3-oxo-3,4-dihydropyrazine-2-carboxylic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 4-(3,4-difluorobenzyl)-3-oxo-3,4-dihydropyrazine-2-carboxylate (110 mg, 0.39 zmol) was placed in a 10-mL RBF and dissolved in THF (3 mL). NaOH (1 mL, 2.000 mmol) (2N solution) was added, and the reaction was allowed to stir at room temp. The reaction was then left stirring overnight at room temp and then analyzed by LC-MS, showing the reaction to be complete. The reaction was then neutralized with the addition of 1N HCl (2 mL), and then saturated with saturated sodium chloride. The resultant mixture was then washed with ethyl acetate (3×50 mL), and then combined organic layers were washed with brine (25 mL) and concentrated in vacuo, affording 4-(3,4-difluorobenzyl)-3-oxo-3,4-dihydropyrazine-2-carboxylic acid as a yellow solid. LRMS (ESI) calc'd for (C12H9F2N2O3) [M+H]+, 267.1; found 267.0.

후처리

  1. waitThe reaction was then left
  2. stirringstirring overnight at room temp
  3. customthe reaction
  4. washThe resultant mixture was then washed with ethyl acetate (3×50 mL)
  5. washcombined organic layers were washed with brine (25 mL)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-25db6904d2fb4d96a1fa0593a2d044ef
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552019B2

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