4-Phenoxyphenyl propargyl ether → 6-phenoxy-2H-1-benzopyran
反応式
[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:7][CH:6]=1)[C:2]#[CH:3]>C(N(CC)C1C=CC=CC=1)C>[O:11]([C:8]1[CH:9]=[CH:10][C:5]2[O:4][CH2:1][CH:2]=[CH:3][C:6]=2[CH:7]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1参加物
3
反応条件
- 温度
- 220 °C
実験手順
4-Phenoxyphenyl propargyl ether (33.7 g, 150 mmol) in 50 mL of N,N-diethylaniline is added to refluxing (220° C.) N,N-diethylanile (300 ml) dropwise over a period of 10 minutes under nitrogen. The mixture is stirred at reflux for 8 hours, cooled and evaporated under high vacuum (bath temp. ~80° C.) to remove solvents. The residue is distilled to give 6-phenoxy-2H-1-benzopyran; b.p. 147°-150° C./0.5 mmHg.
後処理
- temperatureat reflux for 8 hours
- temperaturecooled
- customevaporated under high vacuum (bath temp. ~80° C.)
- customto remove solvents
- distillationThe residue is distilled
出典と根拠
- ORDレコード
- ord-748a7858fe184cc8bed263fd3a791c92
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05155130
反応ノート
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