Ether hydrochloride → HCID 86718836、化合物
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:15])[CH2:9][CH2:10][Si:11]([CH3:14])([CH3:13])[CH3:12].[ClH:16].C(OCC)C>C(OCC)C>[ClH:16].[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:15])[CH2:9][CH2:10][Si:11]([CH3:14])([CH3:13])[CH3:12]参加物
4
実験手順
To the solution of crude (3) (220 gram, 92.2% HPLC purity) in ethyl ether (450 milliliter), was added saturated hydrochloric acid/ethyl ether solution dropwise at room temperature over 30 minutes. The precipitated solid was filtered, the filter cake was washed with mixed solvent (ethyl ether: n-hexane 1:1 v/v; 400 mL), and dried under high vacuum for 2 hours at room temperature to give the desired product (14) (160 g; yield: 62.4%) as a light tan solid. HPLC purity: 98%; LC-MS: m/z 222 (MH+);
後処理
- filtrationThe precipitated solid was filtered
- washthe filter cake was washed with mixed solvent (ethyl ether: n-hexane 1:1 v/v; 400 mL)
- customdried under high vacuum for 2 hours at room temperature
出典と根拠
- ORDレコード
- ord-e1d8518c6f724ff6b82123c7c3da9c19
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722886B1
反応ノート
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