Ethanol → 4-ethoxy-7H-pyrrolo[2,3-d]pyrimidine
反応式
Cl[C:2]1[C:3]2[CH:10]=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1.[OH-].[K+].[CH2:13]([OH:15])[CH3:14]>>[CH2:13]([O:15][C:2]1[C:3]2[CH:10]=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1)[CH3:14]参加物
4
実験手順
To 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (1, 300 mg, 1.95 mmol) in 3.0 mL of ethanol, potassium hydroxide (226 mg, 4.03 mmol) was added and the reaction was microwaved at 120° C. for 3 hours. The reaction was extracted in ethyl acetate and aqueous saturated ammonium chloride. The organic layer was separated and washed with brine, then dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was recrystallized with methanol to provide the desired compound (47, 213 mg). MS (ESI) [M+H+]+=164.9.
後処理
- customthe reaction was microwaved at 120° C. for 3 hours
- extractionThe reaction was extracted in ethyl acetate
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationthe filtrate concentrated under vacuum
- customThe resulting material was recrystallized with methanol
出典と根拠
- ORDレコード
- ord-f52af7d963fa4cdda4f669ffb041765d
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08153641B2
反応ノート
読み込み中…