Methanol → Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate
反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([I:15])[C:13]=1[OH:14])[C:8]([OH:10])=[O:9])([CH3:4])([CH3:3])[CH3:2].S(=O)(=O)(O)O.[CH3:21]O>C1COCC1>[C:1]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([I:15])[C:13]=1[OH:14])[C:8]([O:10][CH3:21])=[O:9])([CH3:4])([CH3:2])[CH3:3]参加物
5
実験手順
24.7 g (77 mmol) of 3-tert-Butyl-4-hydroxy-5-iodobenzoic acid are dissolved in 500 mL of methanol and 50 mL of THF. 5 mL of concentrated sulfuric acid are added and the reaction medium is refluxed for 18 hours. The reaction medium is concentrated under reduced pressure and then diluted in a dichloromethane/water mixture. The organic phase is washed with water and then concentrated under reduced pressure. A yellow solid is obtained (m=24.1 g; yield=94%; m.p.=67° C.).
後処理
- temperaturethe reaction medium is refluxed for 18 hours
- concentrationThe reaction medium is concentrated under reduced pressure
- additiondiluted in a dichloromethane/water mixture
- washThe organic phase is washed with water
- concentrationconcentrated under reduced pressure
- customA yellow solid is obtained (m=24.1 g; yield=94%; m.p.=67° C.)
出典と根拠
- ORDレコード
- ord-e4e7884f138a499ca72491cd93585629
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07468457B2
反応ノート
読み込み中…