Barbital → 1,3-Di(beta-hydroxy-n-propyl)-5,5-diethylbarbituric acid

HRID 971904

反応式

HRID 971904 の反応式
[CH2:1]1[O:4][CH:2]1[CH3:3].[CH2:5]([C:7]1([CH2:16][CH3:17])[C:12](=[O:13])[NH:11][C:10](=[O:14])[NH:9][C:8]1=[O:15])[CH3:6]>[Cl-].C([N+](CC)(CC)CC)C.CN(C)C=O>[OH:4][CH:2]([CH3:3])[CH2:1][N:11]1[C:12](=[O:13])[C:7]([CH2:5][CH3:6])([CH2:16][CH3:17])[C:8](=[O:15])[N:9]([CH2:1][CH:2]([OH:4])[CH3:3])[C:10]1=[O:14]

参加物

5

反応物 2

HCID 2294BarbitalHCID 6378Propylene Oxide

生成物 1

HCID 233382161,3-Di(beta-hydroxy-n-propyl)-5,5-diethylbarbituric acid収率 102.7%

試薬・触媒・溶媒 2

HCID 5946Tetraethylammonium Chloride触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

40.7 g (0.7 mol) of propene oxide are added dropwise over the course of 1 hour to a mixture of 55.3 g of 5,5-diethylbarbituric acid (0.3 mol), 2.77 g of tetraethylammonium chloride (5 mol per cent) and 400 ml of dimethylformamide at 35° C. whilst stirring. Thereafter the mixture is gradually heated to 100° C. After 7 hours' stirring at 100° C. the mixture is worked-up in accordance with example 1. 92.5 g of crude 1,3-di(β-hydroxy-n-propyl)-5,5-diethylbarbituric acid (99.5 % of theory) are obtained. The product boils at 138°-148° C. under 0.08 mm Hg; 75.2 g of pure product 80% of theory) are obtained.

後処理

  1. stirringAfter 7 hours' stirring at 100° C. the mixture

出典と根拠

ORDレコード
ord-7a2066a9bdbc4db68fbd2fa64c2f5a8b
出典データセット
uspto-grants-1979_07
特許番号
US04161594

関連ノート

読み込み中…