Hydrochloric Acid → HCID 19008983、化合物

HRID 1742216ノート

反応式

HRID 1742216 の反応式
Cl.Cl[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH:18]2C(=O)NC(=O)NC2=O)=[CH:12][CH:11]=1.[OH-].[Na+].Cl>O>[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH2:18][C:3]2[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=2)=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 818524-Chloropyridine hydrochlorideHCID 190089865-[2-(4-Chlorophenyl)ethyl]-2,4,6(1H,3H,5H)-pyrimidinetrione

生成物 1

HCID 19008983HCID 19008983、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
200 °C

実験手順

A mixture of 3 g (0.02 m) of 4-chloropyridine hydrochloride and 5.3 g (0.02 m) of 5-[2-(4-chlorophenyl)-ethyl]barbituric acid was thoroughly mixed with a mortar and pestle, heated in a 200° C. oil bath for 15-20 minutes, and then cooled. To the resulting product was added 5 g of NaOH and 40 mL of water, and the mixture was refluxed for several hours. After cooling the mixture, it was acidified with concentrated HCl, again refluxed for 45 minutes, and then cooled. The resulting material was diluted into water; the pH of the aqueous solution was adjusted to 7-8 with dilute NaOH; then the product was extracted into CH2Cl2. The CH2Cl2 layer was separated, filtered through phase separating paper, and concentrated. The residue was adsorbed onto silica gel and chromatographed using 5% EtOAc/CH2Cl2 >10% EtOAc/CH2Cl2 >5% MeOH/EtOAc (wash). Yield 0.82 g.

後処理

  1. additionwas thoroughly mixed with a mortar and pestle
  2. temperaturecooled
  3. temperaturethe mixture was refluxed for several hours
  4. temperatureAfter cooling the mixture, it
  5. temperatureagain refluxed for 45 minutes
  6. temperaturecooled
  7. extractionthen the product was extracted into CH2Cl2
  8. customThe CH2Cl2 layer was separated
  9. filtrationfiltered through phase
  10. customseparating paper
  11. concentrationconcentrated
  12. customchromatographed

出典と根拠

ORDレコード
ord-f37793c340a24ff18d3df026e17947e7
出典データセット
uspto-grants-1994_08
特許番号
US05338742

反応ノート

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