Water → HCID 12291568、化合物
反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][CH:3]=1.[NH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.O>C(Cl)Cl>[N:10]1([CH2:8][C:5]2[CH:6]=[CH:7][N:2]=[CH:3][CH:4]=2)[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1参加物
5
実験手順
A suspension of 4-picolyl chloride hydrochloride (10.0 g, 60.98 mmol) in 100 ml of methylene chloride at room temperature is treated with morpholine (26.52 g, 304.9 mmol, 5.0 equiv.) at once. After stirring for 50 h, the reaction mixture is poured into 250 ml of water, extracted six times with ethylacetate, three times with ethylacetate-methanol (9:1) and the combined organic extracts are dried over Na2SO4. The concentrated filtrate is chromatographed with 350 g of silica gel, packed and eluted with acetone-methylene chloride (1:2), to give 9.17 g (84%) of 4-(4-morpholinyl)methylpyridine as a yellow liquid.
後処理
- extractionextracted six times with ethylacetate, three times with ethylacetate-methanol (9:1)
- dry with materialthe combined organic extracts are dried over Na2SO4
- customThe concentrated filtrate is chromatographed with 350 g of silica gel
- washeluted with acetone-methylene chloride (1:2)
出典と根拠
- ORDレコード
- ord-95f5d281d4cc4aafbe0100df9d5b592e
- 出典データセット
- uspto-grants-2000_03
- 特許番号
- US06043248
反応ノート
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