Methanol → Methyl 4-Iodo-3-methylbenzoate
反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([O:7][CH3:17])=[O:6]参加物
4
実験手順
24.4 g (0.093 mol) of 3-methyl-4-iodobenzoic acid and 250 ml of methanol were introduced into a round-bottomed flask and 2.5 ml of concentrated sulfuric acid were added dropwise. The mixture was heated at reflux for twelve hours, the reaction medium evaporated, taken up in ethyl acetate and water, the organic phase decanted off, dried over magnesium sulfate and evaporated. The residue was triturated in methanol and filtered; 21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered.
後処理
- temperatureThe mixture was heated
- temperatureat reflux for twelve hours
- customthe reaction medium evaporated
- customwater, the organic phase decanted off
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe residue was triturated in methanol
- filtrationfiltered
- custom21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered
出典と根拠
- ORDレコード
- ord-9664b54f4f6141978a503b896b8ef7fd
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723499
反応ノート
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