4-Aminopyridine → HCID 59427333、化合物

HRID 503580ノート

反応式

HRID 503580 の反応式
[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[O:3]1.[CH:11](OCC)(OCC)OCC.[N:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][CH:22]=1>CCCCCC>[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[C:5](=[CH:11][NH:27][C:24]2[CH:25]=[CH:26][N:21]=[CH:22][CH:23]=2)[C:4](=[O:9])[O:3]1

参加物

5

反応物 3

HCID 17274-AminopyridineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformate

生成物 1

HCID 59427333HCID 59427333、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
100 °C

実験手順

In a dried 2-necked RBF equipped with reflux condenser and inert atmosphere, 2,2-dimethyl-1,3-dioxane-4,6-dione (2.33 g, 16 mmol) was dissolved in triethyl orthoformate (16 ml, 97 mmol) and the mixture was stirred at 100° C. under nitrogen for 1.5 h. On complete consumption of starting material (tic), pyridin-4-amine (1.5 g, 16 mmol) was added and heating continued for 4.5 h. The reaction mixture was cooled down to RT and poured into hexane (50 mL). The solid was filtered off and washed with hexane to afford 2,2-dimethyl-5-((pyridin-4-ylamino)methylene)-1,3-dioxane-4,6-dione as an orange solid.

後処理

  1. customIn a dried 2-necked RBF equipped
  2. temperaturewith reflux condenser
  3. additionwas added
  4. temperatureheating
  5. waitcontinued for 4.5 h
  6. temperatureThe reaction mixture was cooled down to RT
  7. filtrationThe solid was filtered off
  8. washwashed with hexane

出典と根拠

ORDレコード
ord-314c85287e93453d8b55b4955e16f06e
出典データセット
uspto-grants-2010_08
特許番号
US07776857B2

反応ノート

読み込み中…