Benzyl 2-(2-pyridyloxy)-2-methylbutanoate → HCID 22270592、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][C:8]([CH3:21])([CH2:19][CH3:20])[C:9]([O:11]CC1C=CC=CC=1)=[O:10]>[Pd].CO>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][C:8]([CH3:21])([CH2:19][CH3:20])[C:9]([OH:11])=[O:10]参加物
4
実験手順
A mixture of benzyl 2-(2-pyridyloxy)-2-methylbutanoate (1.6 g, 5.5 mmol) and 10% palladium on carbon (50 mg) in 50 mL MeOH was degassed and filled with hydrogen using a balloon. After stirring at room temperature overnight, the reaction mixture was filtered through CELITE diatomaceous earth and washed with MeOH (20 mL), and the filtrate was concentrated to dryness to give the title compound. 1H NMR (500 MHz, CD3OD): δ 8.03 (dd, 1H), 7.64 (ddd, 1H), 6.89 (dd, 1H), 6.76 (dd, 1H), 2.14 (m, 1H), 1.94 (m, 1H), 1.64 (s, 3H), 0.99 (t, 3H). LC-MS: m/e 196 (M+H)+ (1.8 min).
後処理
- customwas degassed
- additionfilled with hydrogen using a balloon
- filtrationthe reaction mixture was filtered through CELITE diatomaceous earth
- washwashed with MeOH (20 mL)
- concentrationthe filtrate was concentrated to dryness
出典と根拠
- ORDレコード
- ord-a74d23f5a502486689db0c8951508467
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07550489B2
反応ノート
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