Chloropyrazine → HCID 44325872, 화합물

HRID 378229

반응식

HRID 378229 반응식
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][C@H:3]1[CH2:7][OH:8].CC(C)([O-])C.[K+].Cl[C:16]1[CH:21]=[N:20][CH:19]=[CH:18][N:17]=1>C1COCC1>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][C@H:3]1[CH2:7][O:8][C:16]1[CH:21]=[N:20][CH:19]=[CH:18][N:17]=1

참가 물질

5

반응물 3

HCID 73277ChloropyrazineHCID 643492(2S)-1-Methyl-2-pyrrolidinemethanolHCID 23665647Potassium tert-butoxide

생성물 1

HCID 44325872HCID 44325872, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of (S)-1-methyl-2-pyrrolidinemethanol (1.15 g) in THF (45 mL) was treated with potassium tert-butoxide (1.2 g). After 10 min, chloropyrazine was added and the reaction stirred for 1.5 h. The reaction was quenched with 5 N HCl (4 mL) and the solvent evaporated. The residue was suspended in water and extracted with ether. The aqueous fraction was made basic and extracted with CHCl3. The extracts were dried, the solvent evaporated, and the residue purified by radial chromatography eluting with 20%-EtOH-2%--NH4OH--CHCl3 to give (S)-2-(1-methyl-2-pyrrolidinylmethoxy)pyrazine (1.1). The HCl salt crystallized from EtOAc as a white solid, m.p. 121-122° C. (Compound 28)

후처리

  1. customThe reaction was quenched with 5 N HCl (4 mL)
  2. customthe solvent evaporated
  3. extractionextracted with ether
  4. extractionextracted with CHCl3
  5. customThe extracts were dried
  6. customthe solvent evaporated
  7. customthe residue purified by radial chromatography
  8. washeluting with 20%-EtOH-2%

출처 및 근거

ORD 기록
ord-a97500dcfe004e03807b7b74d83d48f4
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06030966

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