反応式
[O:1]=[C:2]1[C:6]([C:7]([O:9]CC)=O)=[CH:5][C:4]2([CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[O:3]1.[NH2:17][C:18]1[CH2:23][C:22]([CH3:25])([CH3:24])[CH2:21][C:20](=[O:26])[CH:19]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C(OC(=O)C)C>[OH:9][C:7]1[C:6]2[C:2](=[O:1])[O:3][C:4]3([CH2:12][CH2:13][O:14][CH2:15][CH2:16]3)[C:5]=2[C:19]2[C:20](=[O:26])[CH2:21][C:22]([CH3:25])([CH3:24])[CH2:23][C:18]=2[N:17]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 200 °C
実験手順
10 g Ethyl 2-oxo-1,8-dioxaspiro[4.5]dec-3-ene-3-carboxylate and 6.15 g 3-amino-5,5-dimethylcyclohex-2-enone are mixed and heated to 200° C. for 20 minutes under a vacuo of 20 mbar. The mixture is cooled to room temperature and dissolved in 100 ml ethylacetate. 10 g 2,3-dichloro-5,6-dicyano-p-benzoquinone are added and the mixture is stirred for 4 hours at 50° C. and for 18 hours at room temperature. The product is isolated by filtration and washed with ethylacetate.
後処理
- temperatureThe mixture is cooled to room temperature
- customThe product is isolated by filtration
- washwashed with ethylacetate
出典と根拠
- ORDレコード
- ord-ccfd95e97fd24f088bf05e0ba45c9dcf
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029544B2
関連ノート
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