N-methylhydroxylamine hydrochloride → 5,6,7,8-Tetrahydro-7-(N-hydroxymethylamino)quinoline
反応式
[N:1]1[C:10]2[CH:9]=[CH:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.[CH3:12][NH:13]O.C(=O)(O)[O-:16].[Na+]>CO>[OH:16][CH2:12][NH:13][CH:8]1[CH2:9][C:10]2[N:1]=[CH:2][CH:3]=[CH:4][C:5]=2[CH2:6][CH2:7]1参加物
5
実験手順
A solution of 5,6-dihydroquinoline (9.17g, 0.07 mmol) in methanol (10 ml) at 0° was treated portionwise with N-methylhydroxylamine hydrochloride (11.5 g, 0.138 mmol), stirred for 2h, poured into saturated aqueous sodium bicarbonate (250 ml), and extracted with chloroform (3 x 150 ml). The extracts were washed with water (50 ml), dried (MgSO4), and evaporated in vacuo. The residual brown liquid was purified by chromatography (alumina; ether) to give the product (6.45 g) as a colorless oil, which was converted into the amine of Example 2.
後処理
- extractionextracted with chloroform (3 x 150 ml)
- washThe extracts were washed with water (50 ml)
- dry with materialdried (MgSO4)
- customevaporated in vacuo
- customThe residual brown liquid was purified by chromatography (alumina; ether)
出典と根拠
- ORDレコード
- ord-03cc54b39203460baca6abf6253fee61
- 出典データセット
- uspto-grants-1991_12
- 特許番号
- US05075303
反応ノート
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