反応式
[C:1]1([CH:7]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:8](O)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)[Cl:20]>>[C:1]1([CH:7]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:8]([Cl:20])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
実験手順
25 g of 2,3-diphenylpropanoic acid was dissolved in 80 mL of SOCl2 (10 eq.). The reaction mixture was stiffed under N2 overnight at room temperature. Extra SOCl2 removed by evaporation. 2,3-Diphenylpropionylchloride (28 g) was obtained as an oil and used without purification. N-(di-BOC-Amidino)-N′-(2,3-diphenylpropionyl)-1,3-diaminoxylene (5′) To a precooled solution (0° C.) of 3 (27.4 g, 72.3 mmol) in 300 mL of CHCl3, Et3N (7.3 g, 72.3 mmol) and 2,3 diphenylpropionylchloride (17.6 g, 72.3 mmol) was added. The mixture was stirred for 1 hour at room temperature. The solution was washed with water and brine and concentrated to dryness. The crude residue was dissolved in minimum amount of EtOAc and 300 mL of hexane was added. 5 (30.1 g, 71% yield) was collected as a white precipitate.
後処理
- customExtra SOCl2 removed by evaporation
出典と根拠
- ORDレコード
- ord-708600cdccc0423db30e24dcc72f8c8d
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06849733B1
関連ノート
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