Ammonia → HCID 20393354、化合物
反応式
[CH2:1]([N:3]([CH2:27][CH3:28])[CH2:4][CH2:5][N:6]([CH3:26])[C:7](=[O:25])[C:8]([C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=1[C:17](=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O)[CH3:2].N.C([BH3-])#[N:31].[Na+]>>[ClH:16].[CH2:1]([N:3]([CH2:27][CH3:28])[CH2:4][CH2:5][N:6]([CH3:26])[C:7]([C:8]1[NH:31][C:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:11]2[C:10]=1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12]2)=[O:25])[CH3:2]参加物
4
実験手順
In accordance with the procedure described in Example 3, 16.0 g. of o-benzoyl-p-chlorophenylglyoxylic acid [2-(diethylamino)ethyl]methylamide are reacted with 4.1 g. of ammonia and 1.6 g. of sodium cyanoborohydride. The ether extract containing the free base is concentrated to about 300 ml. and treated with ethereal hydrochloric acid. The precipitated hydrochloride is recrystallized from ethanol, and there is obtained 5-chloro-3-phenylisoindole-1-carboxylic acid [2-(diethylamino)ethyl]methylamide hydrochloride in the form of felt-like greenish crystals having a melting point of 208°-210° C. (decomposition).
後処理
- extractionThe ether extract
- additioncontaining the free base
- concentrationis concentrated to about 300 ml
- additionand treated with ethereal hydrochloric acid
- customThe precipitated hydrochloride is recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-729e83bffcb14033ab91796ea797da8f
- 出典データセット
- uspto-grants-1979_09
- 特許番号
- US04167632
反応ノート
読み込み中…