Water → HCID 68598110、化合物
反応式
[CH2:1]1[C:9]2[CH:8]=[C:7]([C:10](OCC)=[O:11])[N:6]=[CH:5][C:4]=2[CH2:3][O:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>C1COCC1>[CH2:1]1[C:9]2[CH:8]=[C:7]([CH2:10][OH:11])[N:6]=[CH:5][C:4]=2[CH2:3][O:2]1参加物
6
実験手順
A solution of ethyl 1,3-dihydrofuro[3,4-c]pyridine-6-carboxylate (0.871 g, 4.51 mmol) in THF (20 ml) at −78° C. under argon was treated with LiAlH4 (1M in THF) (4.51 ml, 4.51 mmol) and allowed warm to rt. After 10 min at rt, water (1 ml), 2M aq NaOH (1 ml) and water (1 ml) were sequentially added and the mixture stirred at rt for 0.5 h. The mixture was then filtered through a short pad of Kieselguhr, eluting with THF (50 ml), organic extracts were then evaporated, chromatographed (0-20% methanol/DCM) to give product as an orange oil (66 mg, 10%).
後処理
- filtrationThe mixture was then filtered through a short pad of Kieselguhr
- washeluting with THF (50 ml), organic extracts
- customwere then evaporated
- customchromatographed (0-20% methanol/DCM)
出典と根拠
- ORDレコード
- ord-146ce6543c8642e986ea81f3fc10e28c
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08389524B2
反応ノート
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