反応式
[C:1](#[N:5])/[CH:2]=[CH:3]/[CH3:4].O1CCCC1.[O:11]1[CH2:16][CH2:15][N:14]([CH:17]([C:20]2[CH:25]=[CH:24][C:23]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[C:22]([N+:32]([O-:34])=[O:33])[CH:21]=2)[C:18]#[N:19])[CH2:13][CH2:12]1.[OH-].[K+]>O.CO>[O:29]1[CH2:30][CH2:31][N:26]([C:23]2[CH:24]=[CH:25][C:20]([C:17]([C:18]#[N:19])([N:14]3[CH2:15][CH2:16][O:11][CH2:12][CH2:13]3)[CH:3]([CH3:4])[CH2:2][C:1]#[N:5])=[CH:21][C:22]=2[N+:32]([O-:34])=[O:33])[CH2:27][CH2:28]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 8.0 parts of crotononitrile in 20 parts by volume of tetrahydrofuran is added to a stirred mixture of 16.5 parts of α-morpholino-α(4-morpholino-3-nitrophenyl)-acetonitrile in 150 parts by volume of tetrahydrofuran and 1.5 parts of potassium hydroxide in 5 parts by volume of methanol at room temperature under an atmosphere of nitrogen. The reaction mixture is stirred for a further 6 hours, diluted with 500 parts by volume of water and extracted with 4×250 parts by volume of ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated under vacuum. The resulting crude product is triturated with a mixture of 50 parts by volume of ethyl acetate and hexane. The solid product is collected, washed with ethyl acetate and dried at 80° under vacuum to give 4-(4-morpholino-3-nitrophenyl)-4-(cyano)-4-(morpholino)-3-methylbutyronitrile having melting point 175°-177° C.
後処理
- extractionextracted with 4×250 parts by volume of ethyl acetate
- dry with materialThe combined organic extracts are dried over magnesium sulphate
- concentrationconcentrated under vacuum
- customThe resulting crude product is triturated with a mixture of 50 parts by volume of ethyl acetate and hexane
- customThe solid product is collected
- washwashed with ethyl acetate
- customdried at 80° under vacuum
出典と根拠
- ORDレコード
- ord-34f3dbb82e4147ccac19e4dc74d3b950
- 出典データセット
- uspto-grants-1987_10
- 特許番号
- US04699908
関連ノート
読み込み中…