2-Hydroxyisobutyric acid → HCID 15224404、化合物

HRID 1006601ノート

反応式

HRID 1006601 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH2:13][CH:14]([CH3:16])[CH3:15])=[CH:9][CH:8]=[CH:7][CH:6]=2.[OH:17][C:18]([CH3:23])([CH3:22])[C:19](O)=O>O>[CH3:22][C:18]([CH3:23])([C:19]1[N:12]([CH2:13][CH:14]([CH3:16])[CH3:15])[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[N:1]=1)[OH:17]

参加物

4

反応物 2

HCID 116712-Hydroxyisobutyric acidHCID 11298872N4-(2-methylpropyl)quinoline-3,4-diamine

生成物 1

HCID 15224404HCID 15224404、化合物収率 22.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

3-Amino-4-(2-methylpropyl amino)quinoline (28.7 g; 0.133 mol) and 2-hydroxyisobutyric acid (27.8 g; 0.267 mol) were mixed and the mixture was heated at 160° C. for 5 hrs. Water was added to the dark mixture and a green oil formed. The oil was extracted with ether to yield 8.6 g of an oil which contained two products. The mixture was purified by silica gel column chromatography to yield 3.2 g of the intended product. A small amount was recrystallized from ethyl acetate for analysis and characterization. m.p. 156-164° C. Analysis: Calculated: C, 72.1; H, 7.5; N, 14.8. Found: C, 71.9; H, 7.4; N, 14.6.

後処理

  1. customa green oil formed
  2. extractionThe oil was extracted with ether

出典と根拠

ORDレコード
ord-0c5585f8605a49ad8f5de57019901097
出典データセット
uspto-grants-2004_09
特許番号
US06790961B2

反応ノート

読み込み中…