Hydroxyamine hydrochloride → 1H-indole-7-carbaldehyde oxime
反応式
Cl.[NH2:2][OH:3].[NH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]=O)[CH:6]=[CH:5]1>N1C=CC=CC=1>[NH:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]=[N:2][OH:3])[CH:6]=[CH:5]1参加物
4
実験手順
Hydroxylamine hydrochloride (0.574 g) was added portionwise to a solution of 1H-indole-7-carbaldehyde (1 g) in pyridine (5 ml) at RT. The resulting solution was heated to reflux and kept at that temperature for 1 hour. The solvent was evaporated. Ethyl acetate (50 mL) was added and the resulting solution was washed with aqueous hydrochloric acid (0.5 M, 40 mL). The organic fraction was separated and dried over anhydrous magnesium sulfate. The dried solution was concentrated to afford 1H-indole-7-carbaldehyde oxime (D1) as a colorless oil which, upon standing, solidified to give a waxy solid (1.1 g). MS (ES): C9H8N2O requires 160; found 161.1 (M+H+).
後処理
- temperatureThe resulting solution was heated
- temperatureto reflux
- customThe solvent was evaporated
- additionEthyl acetate (50 mL) was added
- washthe resulting solution was washed with aqueous hydrochloric acid (0.5 M, 40 mL)
- customThe organic fraction was separated
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe dried solution was concentrated
出典と根拠
- ORDレコード
- ord-5a548ac4f3c84a0a8fbe60225ab04f3a
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08217028B2
反応ノート
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