Acetic acid--water (1/1) → 7-Oxaspiro[3.5]nonan-2-one
反応式
Cl[C:2]1(Cl)[C:5]2([CH2:10][CH2:9][O:8][CH2:7][CH2:6]2)[CH2:4][C:3]1=[O:11].C(O)(=O)C.O>CCOCC.[Zn]>[CH2:4]1[C:5]2([CH2:10][CH2:9][O:8][CH2:7][CH2:6]2)[CH2:2][C:3]1=[O:11]参加物
5
実験手順
The impure 1,1-dichloro-7-oxaspiro[3.5]nonan-2-one from Step B was stirred with zinc (150 mg; 2.30 mmol) and 5 mL of acetic acid/water (1:1) for 4 hours. The mixture was stored at −20° C. for 1 day, diluted with ether (20 mL) and filtered through a pad of Celite®. The solution was neutralized with aqueous sodium bicarbonate solution and extracted into ether (5×20 mL). The combined ether extracts were dried (sodium sulfate), filtered and concentrated under reduced pressure. The material was purified by chromatography on silica gel, eluting with 1:1 ethyl acetate/hexane to give the product as a colorless oil (61 mg).
後処理
- filtrationfiltered through a pad of Celite®
- extractionextracted into ether (5×20 mL)
- dry with materialThe combined ether extracts were dried (sodium sulfate)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe material was purified by chromatography on silica gel
- washeluting with 1:1 ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-fb38331038d7430397d7267b8568337c
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08962596B2
反応ノート
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