Tetrahydrofuran → (6-Aminopyridin-3-yl)methanol
反応式
P(C[C:6]1[N:11]2C=C(C(O)=O)[N:14]=[C:10]2[CH:9]=[CH:8][CH:7]=1)(O)(O)=O.[O:18]1CCC[CH2:19]1>>[NH2:14][C:10]1[N:11]=[CH:6][C:7]([CH2:19][OH:18])=[CH:8][CH:9]=1参加物
3
実験手順
A 250 mL 3-neck flask equipped with an addition funnel, an argon (Ar) inlet and a stopper was flame dried and cooled to room temperature. Dry tetrahydrofuran (THF, 30 mL) was added to the flask, followed by 1M. lithium aluminum hydride (LAH) in Et2O (16 mL). After cooling the solution to 0° C. with a wet ice/water bath, the product from Example 8 (0.92 g, 6 mmol) suspended in THF (100 mL) was added dropwise. The reaction was allowed to warm to room temperature and stir for 3 h. The reaction was quenched with H2O, the salts filtered off and the filtrate stripped to give 0.591 g (99%) of title material.
後処理
- customA 250 mL 3-neck flask equipped with an addition funnel, an argon (Ar) inlet
- temperaturea stopper was flame
- customdried
- additionDry tetrahydrofuran (THF, 30 mL) was added to the flask
- temperatureAfter cooling the solution to 0° C. with a wet ice/water bath
- additionwas added dropwise
- temperatureto warm to room temperature
- customThe reaction was quenched with H2O
- filtrationthe salts filtered off
出典と根拠
- ORDレコード
- ord-ca38f39571054032a43dce3d17c5611b
- 出典データセット
- uspto-grants-1998_02
- 特許番号
- US05716964
反応ノート
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