Hydrochloric Acid → 2H,5H-Spiro[imidazolidine-4,5'-indeno[1,2-b]pyridine]-2,5-dione

HRID 485705

反応式

HRID 485705 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[C:7](=O)[C:8]3[C:13]([C:2]=12)=[CH:12][CH:11]=[CH:10][CH:9]=3.[C-]#N.[K+].[C:18](=[O:21])([O-])[O-].[NH4+:22].[NH4+:23].Cl.[CH2:25]([OH:27])C>O>[NH:22]1[C:25](=[O:27])[C:7]2([C:3]3[C:2](=[N:1][CH:6]=[CH:5][CH:4]=3)[C:13]3[C:8]2=[CH:9][CH:10]=[CH:11][CH:12]=3)[NH:23][C:18]1=[O:21]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 9032Potassium CyanideHCID 774895H-Indeno(1,2-b)pyridin-5-oneHCID 517111Ammonium Carbonate

生成物 1

HCID 134913842H,5H-Spiro[imidazolidine-4,5'-indeno[1,2-b]pyridine]-2,5-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
105 °C

実験手順

5H-Indeno[1,2-b]pyridine-5-one (4.0 g, 22 mmol) was mixed with potassium cyanide (1.6 g, 24 mmol) and ammonium carbonate (5.3 g, 55 mmol) in 90% ethanol (75 mL) in a pressure reactor and heated at 105° C. for 40 hr. The mixture was poured into 300 mL of water, acidified with conc. HCl (pH 1), and filtered. The filtrate was neutralized and the solid which formed collected by filtration, washed with water, and dried to yield 4.5 g. This solid was crystallized from ethyl acetate to yield 3.2 g of product. (This material was no longer soluble in ethyl acetate after the first crystallization). m/e30 . 251.

後処理

  1. filtrationfiltered
  2. customthe solid which formed
  3. filtrationcollected by filtration
  4. washwashed with water
  5. customdried
  6. customto yield 4.5 g
  7. customThis solid was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-d9247d14c0314030babc77b9b3c1c949
出典データセット
uspto-grants-1985_08
特許番号
US04537892

関連ノート

読み込み中…