反応式
[CH3:1][C:2]1[N:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.Cl.CN(C)CCCN=C=NCC.ON1C2N=CC=CC=2N=N1.[NH2:37][C:38]1[CH:39]=[CH:40][C:41]([Cl:48])=[C:42]([CH:47]=1)[C:43]([O:45][CH3:46])=[O:44]>CN(C)C=O.O>[CH3:46][O:45][C:43](=[O:44])[C:42]1[CH:47]=[C:38]([NH:37][C:4]([C:3]2[C:2]([CH3:1])=[N:10][C:9]([C:11]([F:14])([F:13])[F:12])=[CH:8][CH:7]=2)=[O:6])[CH:39]=[CH:40][C:41]=1[Cl:48]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of 2-methyl-6-trifluoromethylnicotinic acid (4.77 g; 23 mmol) in dimethyl formamide (100 ml) was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (4.46 g; 23 mmol) and 1-hydroxy-7-azabenzotriazole (3.17 g; 23 mmol) and the resulting solution was stirred at room temperature for 30 minutes. To this was added a solution of methyl 5-amino-2-chlorobenzoate (3.6 g; 19 mmol) in dimethyl formamide (25 ml) and the resulting solution stirred at room temperature for 18 hours. Water (200 ml) was added to the reaction mixture and this was extracted with ethyl acetate (3×200 ml). The combined organic layers were washed with saturated sodium bicarbonate solution (2×300 ml). The organic layer was dried (magnesium sulphate), filtered and evaporated to give 2-chloro-5-[(2-methyl-6-trifluoromethyl-pyridine-3-carbonyl)-amino]-benzoic acid methyl ester (6.6 g, 94%).
後処理
- stirringthe resulting solution stirred at room temperature for 18 hours
- extractionthis was extracted with ethyl acetate (3×200 ml)
- washThe combined organic layers were washed with saturated sodium bicarbonate solution (2×300 ml)
- dry with materialThe organic layer was dried (magnesium sulphate)
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-cc6abcabe9744b53a82442c649187893
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07816369B2
関連ノート
読み込み中…