Chloropyrazine → HCID 44325872、化合物

HRID 378229

反応式

HRID 378229 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 44325872HCID 44325872、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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)

後処理

  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%

出典と根拠

ORDレコード
ord-a97500dcfe004e03807b7b74d83d48f4
出典データセット
uspto-grants-2000_02
特許番号
US06030966

関連ノート

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