反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][C:11]([OH:13])=O.[N:14]1C=CC=CC=1.C(OC(OC(C)(C)C)=O)(OC(C)(C)C)=O.C(=O)([O-])O.[NH4+]>C(#N)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][C:11]([NH2:14])=[O:13]参加物
実験手順
3-(2-methoxyphenyl)propionic acid (9.0 g, 49.9 mmol) was dissolved in acetonitrile (10 mL). Subsequently, pyridine (3.54 g, 44.9 mmol) and di-tert-butyl dicarbonate [Boc2O (16.3 g, 74.85 mmol)] were added thereto. The mixture was stirred for 10 minutes at room temperature, and then ammonium hydrogencarbonate (5.92 g, 74.9 mmol) were added. After completion of reaction, the reaction mixture was concentrated under reduced pressure. Thereafter, the resultant concentrate was added to water, and the resultant mixture was extracted with chloroform, followed by washing sequentially with 1M hydrochloric acid and saturated brine. The resultant mixture was subjected to drying over magnesium sulfate and concentration under reduced pressure. The resultant concentrate was used in Production Example 36 without purification.
後処理
- customAfter completion of reaction
- concentrationthe reaction mixture was concentrated under reduced pressure
- concentrationThereafter, the resultant concentrate
- additionwas added to water
- extractionthe resultant mixture was extracted with chloroform
- washby washing sequentially with 1M hydrochloric acid and saturated brine
- dry with materialto drying over magnesium sulfate and concentration under reduced pressure
- concentrationThe resultant concentrate
- customwas used in Production Example 36 without purification
出典と根拠
- ORDレコード
- ord-f1e930a46d5e40c7b88bebef76659de2
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06653334B1
関連ノート
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