Potassium Hydroxide → 2-Cyclohexylideneacetic acid
反応式
[OH-].[K+].C([O:5][C:6](=[O:14])[CH:7]=[C:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)C>O.CO>[C:8]1(=[CH:7][C:6]([OH:14])=[O:5])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1参加物
5
実験手順
A mixture of KOH (1.0 g, 18 mmol) dissolved in water (25 mL) and Intermediate 3 (1.6 g, 9.5 mmol) dissolved in MeOH (5 mL) was stirred for 18 hours at room temperature. The reaction was refluxed for one hour, cooled, then extracted with EtOAc. The aqueous layer was acidified with 1N NCl and extracted with EtOAc, washed with brine, dried (Na2SO4), and concentrated in vacuo to provide 1.3 g (100%) of Intermediate 4. 1H NMR (DMSO-d6) δ: 1.55 (br s, 6H) 2.1 (m, 2H), 2.8 (m, 2H), 5.5 (s, 1H), 11.9 (s, 1H); MS ES−m/e 139.1 (p−1).
後処理
- temperatureThe reaction was refluxed for one hour
- temperaturecooled
- extractionextracted with EtOAc
- extractionextracted with EtOAc
- washwashed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-965e90e91c0f4179825256b49f9ee004
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07122554B2
反応ノート
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