Ethanolamine → 2-((6-Chloropyrazin-2-yl)amino)ethanol
反応式
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[NH2:9][CH2:10][CH2:11][OH:12].CCN(C(C)C)C(C)C>C(O)CCC>[Cl:8][C:4]1[N:3]=[C:2]([NH:9][CH2:10][CH2:11][OH:12])[CH:7]=[N:6][CH:5]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
In a sealed tube, 2,6-dichloropyrazine (1 g, 6.71 mmol) was mixed with 2-aminoethanol (0.492 g, 8.05 mmol), Hunig's base (1.13 g, 8.73 mmol) in BuOH (7 mL) and the reaction mixture was heated to 80° C. over night. The mixture was concentrated in vacuo and the residue partitioned between NaHCO3 (20 mL) and EtOAc (100 mL). The organic phase was separated, washed with brine, dried over Na2SO4, filtered and evaporated to dryness to give the title compound (0.583 g, 50%) as a light yellow foam. MS: 174.1 (M+H+).
後処理
- concentrationThe mixture was concentrated in vacuo
- customthe residue partitioned between NaHCO3 (20 mL) and EtOAc (100 mL)
- customThe organic phase was separated
- washwashed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-0651662b5f2445acb5803f7bbfa2290b
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09260408B2
反応ノート
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