Hydroxyamine hydrochloride → HCID 75103735、化合物
反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:11])=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=O.[NH2:12][OH:13].Cl>C(O)C.O>[CH3:1][O:2][C:3]1[C:4]([CH3:11])=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=[N:12][OH:13]参加物
5
実験手順
To an ice-cooled and stirred suspension of 3-methoxy-2-methylbenzaldehyde (0.269 g, 1.8 mmol) in ethanol (15 ml) a solution of NaOAc.3H2O (1.3 eq) and NH2OH.HCl (1.3 eq) in water (5 ml) was added dropwise within 5 minutes. The resulting suspension was stirred at room temperature until the starting material was consumed (monitored by TLC). After evaporation of the ethanol in vacuo, water was added to the residue. Then the precipitated crystals were filtered off. The crude product was purified by column chromatography with a mixture of chloroform:ethyl acetate (95:5) as the eluent.
後処理
- additionwas added dropwise within 5 minutes
- stirringThe resulting suspension was stirred at room temperature until the starting material
- customwas consumed (monitored by TLC)
- customAfter evaporation of the ethanol in vacuo, water
- additionwas added to the residue
- filtrationThen the precipitated crystals were filtered off
- customThe crude product was purified by column chromatography with a mixture of chloroform:ethyl acetate (95:5) as the eluent
出典と根拠
- ORDレコード
- ord-7110f1ee85b549b895d76688602304b6
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536210B2
反応ノート
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