反応式
Cl.[C:2]([C:6]1[CH:7]=[C:8]([CH:18]=[CH:19][CH:20]=1)[O:9][CH2:10][CH2:11][CH:12]1[O:17]CCCO1)([CH3:5])([CH3:4])[CH3:3]>C1COCC1>[C:2]([C:6]1[CH:7]=[C:8]2[C:18]([CH:12]([OH:17])[CH2:11][CH2:10][O:9]2)=[CH:19][CH:20]=1)([CH3:3])([CH3:4])[CH3:5]参加物
4
実験手順
Concentrated hydrochloric acid (70 mL) was cooled in an ice bath and then about 40 mL of THF was added and stirred. At 0° C. with stirring was added 2-[2-(3-tert-Butyl-phenoxy)-ethyl]-[1,3]dioxane (8.48 g, 32.1 mmol) slowly in THF (30 mL). After the addition was complete the ice bath was removed and the resulting mixture was stirred vigorously at room temperature for 3 hours. Then ether was added (300 mL) and the layers were separated, and the organic layer was extracted with water (3×100 mL) and finally dried over magnesium sulfate, filtered and concentrated to give the title compound as a light yellow oil and used for the next step without further purification.
後処理
- stirringAt 0° C. with stirring
- additionAfter the addition
- customwas removed
- stirringthe resulting mixture was stirred vigorously at room temperature for 3 hours
- additionThen ether was added (300 mL)
- customthe layers were separated
- extractionthe organic layer was extracted with water (3×100 mL)
- dry with materialfinally dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-314583de2bf14be681b887716cef27fd
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08318719B2
関連ノート
読み込み中…