反応式
[O:1]1[CH2:5][CH2:4][CH:3]([CH:6]=O)[CH2:2]1.[C:8]([O:12][C:13]([NH:15][CH2:16][CH2:17][NH:18][CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=1)=[O:14])([CH3:11])([CH3:10])[CH3:9].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].S([O-])([O-])(=O)=O.[Mg+2]>ClCCCl>[C:8]([O:12][C:13]([NH:15][CH2:16][CH2:17][N:18]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=1)[CH2:6][CH:3]1[CH2:4][CH2:5][O:1][CH2:2]1)=[O:14])([CH3:11])([CH3:10])[CH3:9]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
This compound was made in a manner analogous to that set forth in Step D of Example 5, using 0.2 gram (0.0020 mole) of (oxolan-3-yl)formaldehyde, 0.56 gram (0.0020 mole) of (tert-butoxy)-N-(2-{[(4-methoxyphenyl)methyl]amino}-ethyl)carboxamide (prepared in Step A of Example 9), 0.64 gram (0.0030 mole) of sodium triacetoxyborohydride and 2.5 grams (0.021 mole) of magnesium sulfate in 50 mL of 1,2-dichloroethane. The reaction product was purified with column chromatography on silica gel. Elution was accomplished using a mixture of 1% methanol in methylene chloride as an eluant. Appropriate fractions were combined and concentrated under reduced pressure, yielding 0.59 gram of the subject compound. The NMR spectrum was consistent with the proposed structure.
後処理
- customThe reaction product was purified with column chromatography on silica gel
- washElution
- additiona mixture of 1% methanol in methylene chloride as an eluant
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-ab9d4328df8b41dcbeb9a02578764ec8
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07977332B2
関連ノート
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