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

HRID 485705

반응식

HRID 485705 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
105 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d9247d14c0314030babc77b9b3c1c949
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04537892

연결된 노트

불러오는 중…