Hydrochloric Acid → HCID 19374875、化合物
反応式
Cl.C([NH:10][C:11](=[S:25])[N:12]([CH:16]([C:18]1[CH:23]=[CH:22][N:21]=[CH:20][C:19]=1[Cl:24])[CH3:17])[CH2:13][CH2:14][CH3:15])(=O)C1C=CC=CC=1>O>[Cl:24][C:19]1[CH:20]=[N:21][CH:22]=[CH:23][C:18]=1[CH:16]([N:12]([CH2:13][CH2:14][CH3:15])[C:11]([NH2:10])=[S:25])[CH3:17]参加物
4
実験手順
Add 6 ml of 32% hydrochloric acid to 1.18 g of the compound obtained in Step A. Bring the reaction medium to 80° C. for one hour, then cool and add water. Extract with methylene chloride and discard the organic phase. Alkanilise the aqueous phase with sodium carbonate and extract with methylene chloride. Dry the organic phase and evaporate under vacuum. Purify the residue by chromatography on a silica column, using a mixture of methylene chloride and methanol (98:2 V/V) as eluent.
後処理
- temperaturecool
- extractionExtract with methylene chloride
- extractionAlkanilise the aqueous phase with sodium carbonate and extract with methylene chloride
- customDry the organic phase
- customevaporate under vacuum
- customPurify the residue by chromatography on a silica column
- additiona mixture of methylene chloride and methanol (98:2 V/V) as eluent
出典と根拠
- ORDレコード
- ord-0a6fbf346934482d880efff9a5832b05
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05464847
反応ノート
読み込み中…