反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH:9]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[C:10]#[N:11])[CH:4]=1.[OH-].[K+].C(O)C.[C:25](#[N:29])/[CH:26]=[CH:27]/[CH3:28]>O1CCCC1>[CH3:28][CH:27]([CH2:26][C:25]#[N:29])[C:9]([N:12]1[CH2:13][CH2:14][O:15][CH2:16][CH2:17]1)([C:5]1[CH:4]=[C:3]([C:2]([F:1])([F:18])[F:19])[CH:8]=[CH:7][CH:6]=1)[C:10]#[N:11]参加物
5
実験手順
To a solution of α-(α,α,α-trifluoro-m-tolyl)-4-morpholineacetonitrile in 100 ml. of tetrahydrofuran is added 1.0 ml. of 30% KOH-ethanol solution. To the mixture is added 2.56 g. of crotononitrile and the mixture is stirred at room temperature for 18 hrs. The mixture is concentrated to dryness under vacuum and the residue is dissolved in chloroform. The solution is passed through a column of hydrous magnesium silicate. The eluent is concentrated to an oil (17.3 g) which is crystallized from hexane and recrystallized from CHCL3 -hexane to give 3-methyl-2-morpholino-2-(α,α,α-trifluoro-m-tolyl)glutaronitrile as crystals, m.p. 115°-118° C.
後処理
- additionTo the mixture is added 2.56 g
- concentrationThe mixture is concentrated to dryness under vacuum
- dissolutionthe residue is dissolved in chloroform
- concentrationThe eluent is concentrated to an oil (17.3 g) which
- customis crystallized from hexane
- customrecrystallized from CHCL3 -hexane
出典と根拠
- ORDレコード
- ord-6baa0556377e44a7821e68c108ea8bbc
- 出典データセット
- uspto-grants-1978_09
- 特許番号
- US04112095
関連ノート
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