反応式
CS(C)=O.C(Cl)(=O)C(Cl)=O.[O:11]([CH2:19][CH2:20][CH2:21][OH:22])[Si:12]([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13].C(N(CC)CC)C.Cl>C(Cl)Cl>[O:11]([CH2:19][CH2:20][CH:21]=[O:22])[Si:12]([C:15]([CH3:17])([CH3:18])[CH3:16])([CH3:14])[CH3:13]参加物
7
反応条件
- 温度
- -78 °C
実験手順
DMSO (24 mmol) is added to oxalyl chloride (11 mmol) in 40 mL of CH2Cl2 cooled to −78° C. After 15 minutes, alcohol 46 (10 mmol) is added. After an additional 15 minutes, triethylamine (50 mmol) is added. The mixture is allowed to warm to 0° C. and then poured into 0.1 M HCl (100 mL). The phases are separated, and the aqueous phase is extracted with ethyl acetate (2×100 mL). The organic phases are washed with water (100 mL), dried over anhydrous MgSO4, and concentrated in vacuo. The mixture is purified by flash chromatography to give the product as a colorless oil.
後処理
- waitAfter an additional 15 minutes
- temperatureto warm to 0° C.
- customThe phases are separated
- extractionthe aqueous phase is extracted with ethyl acetate (2×100 mL)
- washThe organic phases are washed with water (100 mL)
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated in vacuo
- customThe mixture is purified by flash chromatography
出典と根拠
- ORDレコード
- ord-5c15f2fb99da45d49beebf1bfbf5498f
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06702705B1
関連ノート
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