反応式
[Si:1]([O:8][CH2:9][CH:10]1[CH2:12][CH:11]1[CH2:13][CH2:14]O)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:35]Br.C(=O)([O-])O.[Na+]>CN(C)C=O>[Si:1]([O:8][CH2:9][CH:10]1[CH2:12][CH:11]1[CH2:13][CH2:14][Br:35])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]参加物
6
反応条件
- 温度
- -20 °C
実験手順
2-(2-hydroxyethyl)cyclopropylmethyl t-butyldimethylsilyl ether (15.0 g, 65 mmol) was dissolved in N,N-dimethylformamide (120 ml), and triphenylphosphine (17.3 g, 66 mmol) was added thereto at room temperature. Twenty minutes later, the mixture was cooled to -20° C. Bromine (10.5 g, 66 mmol) was added thereto over a period of 5 minutes, and the temperature was gradually raised to 0° C. The mixture was poured into a saturated sodium hydrogen carbonate aqueous solution, and the product was extracted with ethyl ether. Then, it was dried over anhydrous magnesium sulfate and purified by silica gel column chromatography to obtain 2-(2-bromoethyl)cyclopropylmethyl t-butyldimethylsilyl ether (2.7 g).
後処理
- customat room temperature
- temperaturethe temperature was gradually raised to 0° C
- extractionthe product was extracted with ethyl ether
- dry with materialThen, it was dried over anhydrous magnesium sulfate
- custompurified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-d890c419f22941b6b3aede17a4928400
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05416231
関連ノート
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