2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 2-((Propan-2-yl)amino)benzaldehyde
反応式
[CH:1]([NH:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH2:7][OH:8])([CH3:3])[CH3:2].ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[CH:1]([NH:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=[O:8])([CH3:3])[CH3:2]参加物
4
実験手順
To a solution of 9.6 g of 2-isopropylaminobenzyl alcohol in 200 ml of dioxane was added 13.2 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in several portions, followed by stirring for an hour. The solvent was evaporated, the reaction solution was concentrated, and methylene chloride was added thereto, followed by filtration. The filtrate was concentrated, and the resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to give 7.6 g of 2-isopropylaminobenzaldehyde.
後処理
- customThe solvent was evaporated
- concentrationthe reaction solution was concentrated
- additionmethylene chloride was added
- filtrationfollowed by filtration
- concentrationThe filtrate was concentrated
- customthe resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)
出典と根拠
- ORDレコード
- ord-8547a040ad9a425c98f22d4b4c6c403c
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05733917
反応ノート
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