反応式
[Cl:1][C:2]1[C:7]([OH:8])=[C:6]([Cl:9])[CH:5]=[C:4]([CH3:10])[CH:3]=1.[O:11]1[CH2:15][CH2:14]OC1=O>N1C=CN=C1>[Cl:1][C:2]1[CH:3]=[C:4]([CH3:10])[CH:5]=[C:6]([Cl:9])[C:7]=1[O:8][CH2:14][CH2:15][OH:11]参加物
4
反応条件
- 温度
- 160 °C
実験手順
In a three-necked flask equipped with a gas droplet counter and an efficient cooling system, a mixture of 2,6-dichloro-p-cresol (20.0 g, 113 mmol), [1,3]dioxolan-2-one (9.95 g, 113 mmol) and imidazole (115 mg, 1.70 mmol) was heated to 160° C. for 25 h. The mixture was allowed to cool to rt. Purification by FC (Et2O/heptane 1.1) yielded the title compound (18.7 g, 75%). LC-MS: tR=0.88 min.
後処理
- customIn a three-necked flask equipped with a gas droplet counter
- temperatureto cool to rt
- customPurification by FC (Et2O/heptane 1.1)
出典と根拠
- ORDレコード
- ord-7c44d5c67c06435498534780c07c1f13
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07968720B2
関連ノート
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