Diethyl Ether → Methyl 4-iodobenzoate
反応式
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.[CH3:11]COCC.[N+](=C)=[N-]>O1CCCC1>[CH3:11][O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([I:1])=[CH:3][CH:4]=1参加物
5
実験手順
Fifty (50) mmol (12.4 g) of commercially available 4-iodobenzoic acid was dissolved in 200 ml of tetrahydrofuran and then added to an ether solution containing freshly prepared diazomethane. The excess diazomethane was subsequently consumed by addition of glacial acetic acid and the resultant solution was concentrated in vacuo. The residue thus obtained was partitioned between ethyl acetate and saturated NaHCO3. The layers were separated and the aqueous phase was extracted with 100 ml of ethyl acetate. The organic extracts were combined, dried over Na2SO4, and concentrated in vacuo, yielding 13.01 grams (99.3% yield) of a yellow solid which melted at 111° C.
後処理
- customThe excess diazomethane was subsequently consumed by addition of glacial acetic acid
- concentrationthe resultant solution was concentrated in vacuo
- customThe residue thus obtained
- customwas partitioned between ethyl acetate and saturated NaHCO3
- customThe layers were separated
- extractionthe aqueous phase was extracted with 100 ml of ethyl acetate
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-a23a2974ba3941e79b71f0f690cd1e1b
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05726312
反応ノート
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