Hydrochloric Acid → 2-Methyl-2-(phenylsulfanyl)propan-1-ol
反応式
[CH3:1][C:2]([S:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([CH3:7])[C:3](OC)=[O:4].CC(C[AlH]CC(C)C)C.Cl>ClCCl.C1(C)C=CC=CC=1>[CH3:7][C:2]([S:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([CH3:1])[CH2:3][OH:4]参加物
6
実験手順
A −78° C. solution of Example 103B (860 mg, 4.1 mmol) in dichloromethane (10 mL) was treated with 1.0M DIBAL-H in toluene (11 mL), warmed to room temperature over 4 hours, poured into a mixture of 3M HCl (15 mL) and ice (˜10 g), and extracted with ethyl acetate (100 mL). The combined extracts were washed with 1M HCl (10 mL) and brine (10 mL), dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 10-30% ethyl acetate/hexanes to provide the desired product. MS (DCI) m/e 183 (M+H)+.
後処理
- extractionextracted with ethyl acetate (100 mL)
- washThe combined extracts were washed with 1M HCl (10 mL) and brine (10 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe concentrate was purified by flash column chromatography on silica gel with 10-30% ethyl acetate/hexanes
出典と根拠
- ORDレコード
- ord-03ba32d8eed0482b8a2708b967f374ff
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07504512B2
反応ノート
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