反応式
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5](Cl)=[O:6].[CH3:12][NH2:13].C1COCC1>C(Cl)Cl>[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([NH:13][CH3:12])=[O:6]参加物
5
実験手順
To a cooled (0° C.) solution of 3-iodo-4-methylbenzoyl chloride (2.80 g; 10.0 mmol) in DCM (10 mL) was slowly added a 2 M solution of methylamine in THF (11 mL, 2.2 eq.). Upon completion of the addition, the ice bath was removed and the mixture was stirred overnight. All volatiles were removed in vacuo and the residue was treated with aq. NaHCO3 (25 mL) and subsequently extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4 and evaporated. The target compound 3-iodo-N,4-dimethylbenzamide (2.62 g, 95% yield) was used without further purification.
後処理
- additionUpon completion of the addition
- customthe ice bath was removed
- customAll volatiles were removed in vacuo
- additionthe residue was treated with aq. NaHCO3 (25 mL)
- extractionsubsequently extracted with ethyl acetate (3×15 mL)
- dry with materialThe combined organic layers were dried over MgSO4
- customevaporated
出典と根拠
- ORDレコード
- ord-4d373b660c0a44c5833c706f21fb3554
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642611B2
関連ノート
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