反応式
[O:1]=[C:2]([NH:11][NH:12][C:13]([N:15]1[CH2:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[O:18][C:17]2[CH:26]=[CH:27][C:28]([Cl:30])=[CH:29][C:16]1=2)=[O:14])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][N:6]=1>C(O)C>[ClH:30].[O:1]=[C:2]([NH:11][NH:12][C:13]([N:15]1[CH2:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[O:18][C:17]2[CH:26]=[CH:27][C:28]([Cl:30])=[CH:29][C:16]1=2)=[O:14])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][N:6]=1参加物
実験手順
2.64 g of 8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, 2-[1-oxo-3-(2-pyridinyl)propyl]hydrazide (6), prepared as described above in Example 6, was taken up in 25 mL of 3A ethanol and filtered to remove any undissolved material. The solution was cooled in an ice bath with stirring. To this was added dropwise 5.3 mL of 9.5M hydrogen chloride in ethanol. After stirring in the ice bath for 5 minutes, some of the product precipitated. This was poured slowly into 275 mL of stirring diethyl ether (Et2O), and the resulting mixture was stirred for 5 minutes. The resulting solid product was collected by filtration, washed with 20 mL of 3A ethanol, followed by Et2O, and dried under vacuum at 56° C. to yield 2.20 g (76.7%) of a white powder. Analysis calculated for C22H20N4O3Cl2 : C, 57.53; H, 4.39; N, 12.20; C1, 15.44; Found: C, 57.31; H, 4.36; N, 11.98; Cl, 15.11.
後処理
- filtrationfiltered
- customto remove any undissolved material
- temperatureThe solution was cooled in an ice bath
- additionTo this was added dropwise 5.3 mL of 9.5M hydrogen chloride in ethanol
- stirringAfter stirring in the ice bath for 5 minutes
- customsome of the product precipitated
- additionThis was poured slowly into 275 mL of stirring diethyl ether (Et2O)
- stirringthe resulting mixture was stirred for 5 minutes
- filtrationThe resulting solid product was collected by filtration
- washwashed with 20 mL of 3A ethanol
- customdried under vacuum at 56° C.
出典と根拠
- ORDレコード
- ord-4e66486246b441c5984be034cde871c9
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05464830
関連ノート
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