反応式
[Cl:1][C:2]1[CH:12]=[N:11][C:10]2[O:9][CH:8]([CH2:13][CH2:14]Cl)[CH2:7][N:6]([CH3:16])[C:5](=[O:17])[C:4]=2[CH:3]=1.[C:18](=[O:21])([O-:20])[O-].[K+].[K+].[NH:24]1[CH2:27][CH2:26][CH2:25]1.[OH-:28].[NH4+]>CS(C)=O.O.CO.C(OCC)(=O)C>[C:5]([OH:17])(=[O:28])[C:18]([OH:20])=[O:21].[N:24]1([CH2:14][CH2:13][CH:8]2[CH2:7][N:6]([CH3:16])[C:5](=[O:17])[C:4]3[CH:3]=[C:2]([Cl:1])[CH:12]=[N:11][C:10]=3[O:9]2)[CH2:27][CH2:26][CH2:25]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 4
実験手順
To a solution of 6 g (0.022 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-one in 40 ml of dimethyl sulfoxide was added 8.0 g of crushed potassium carbonate and 1.5 g (0.026 mole) of azetidine. The reaction was stirred at room temperature for 24 hr. After checking ty TLC [7:2:1 by volume ethyl acetate:methanol:conc. ammonium hydroxide, another 0.4 g (0.007 mole) of azetidine was added. Two days later, another 0.5 g (0.0087 mole) of azetidine was added and the mixture stirred for 24 hr more. The reaction mixture was diluted with 100 ml of water and extracted with 4×100 ml of benzene. The organic extracts were combined, washed with 3×100 ml of water, dried over sodium sulfate, filtered, and concentrated by rotary evaporation. The syrupy residue was treated with oxalic acid in isopropyl alcohol. This yielded 4.2 g (56.5%) of white material, m.p. 169°-174° C. with decomposition.
後処理
- stirringthe mixture stirred for 24 hr more
- extractionextracted with 4×100 ml of benzene
- washwashed with 3×100 ml of water
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
- additionThe syrupy residue was treated with oxalic acid in isopropyl alcohol
出典と根拠
- ORDレコード
- ord-c8d4455c6b164a84bffaf46314b5819e
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04727152
関連ノート
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