反応式
[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([Br:14])=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11])(=[O:3])[CH3:2].ON1[C:20]2C=CC=C[C:19]=2N=N1.CN(C1C=CC=CN=1)C.Cl.CN(C)CCCC(N=C=N)C>ClCCl.C(O)C>[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([Br:14])=[C:9]([CH:13]=1)[C:10]([O:12][CH2:19][CH3:20])=[O:11])(=[O:3])[CH3:2]参加物
6
実験手順
A mixture of 5-(acetylamino)-2-bromobenzoic acid (2.58 g, 10 mmol), 1-hydroxybenzotriazole (1.68 g, 11 mmol), dimethylaminopyridine (1.22 g, 10 mmol) and 1-(3-dimethylaminopropyl)-ethylcarbodiimide hydrochloride (2.20 g, 11.5 mmol) in dichloromethane/ethanol (5:1, 30 ml) was stirred at room temperature for 2 hours then washed with saturated sodium bicarbonate solution, dried (magnesium sulphate) and chromatographed on silica eluting with ethyl acetate/iso-hexane (2:3) to give 2.18 g of white solid.
後処理
- washthen washed with saturated sodium bicarbonate solution
- dry with materialdried (magnesium sulphate)
- customchromatographed on silica eluting with ethyl acetate/iso-hexane (2:3)
出典と根拠
- ORDレコード
- ord-943100f8158e4b6f8c445f41bf2972e8
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07446222B2
関連ノート
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