Sodium Hydroxide → HCID 17952314、化合物
反応式
C[O:2][C:3](=[O:17])[CH2:4][CH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][N:6]1[CH:14]([CH3:16])[CH3:15].[OH-].[Na+]>CO>[CH:14]([N:6]1[CH2:7][C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]1[CH2:4][C:3]([OH:17])=[O:2])([CH3:16])[CH3:15]参加物
4
実験手順
To the compound of Step B (0.53 g., 2.30 mmol) in MeOH (5.1 mL) was added 1.0N NaOH (2.53 mL, 2.53 mmol). After two days, the solution was concentrated to dryness. The resulting residue was diluted with 1.0N HCl and water was loaded onto a strong cation exchange resin. The resin was washed with water, TBF/water (1:1) and then water. The product was then eluted from the resin with pyridine/water (1:9). The eluent was concentrated to dryness to afford about 0.43 g (85%) of the final compound. EIS-MS 220 [M+1].
後処理
- concentrationthe solution was concentrated to dryness
- additionThe resulting residue was diluted with 1.0N HCl and water
- washThe resin was washed with water, TBF/water (1:1)
- washThe product was then eluted from the resin with pyridine/water (1:9)
- concentrationThe eluent was concentrated to dryness
出典と根拠
- ORDレコード
- ord-82ed703795084fc9ac27e2d42f8b82c0
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07291619B2
反応ノート
読み込み中…