Histamine → HCID 178526685, 화합물

HRID 726240

반응식

HRID 726240 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH:11]1[N:15]=[CH:14][NH:13][C:12]=1[CH2:16][CH2:17][NH2:18]>CC(O)C>[NH:15]1[CH:11]=[C:12]([CH2:16][CH2:17][NH:18][C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=2)[N:13]=[CH:14]1

참가 물질

4

반응물 2

HCID 774HistamineHCID 783082-Chloro-5-nitropyridine

생성물 1

HCID 178526685HCID 178526685, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

2.22 g (14 mmol) of 2-chloro-5-nitropyridine and an equimolar equivalent of histamine base (1.56 g) in 10 ml of 2-propanol are brought to reflux for 48 h. The reaction mixture is concentrated to dryness and the solid residue is taken up in water, heated to boiling, cooled and filtered. The filtrate is concentrated to dryness and chromatographed on a column of silica gel which is eluted with a mixture of chloroform and methanol (5, 10 and 20%). The combined pure fractions are evaporated to dryness and the solid residue is crystallized from absolute ethanol to provide the product. M.p.: 162°-163° C.

후처리

  1. temperatureto reflux for 48 h
  2. concentrationThe reaction mixture is concentrated to dryness
  3. temperatureheated
  4. temperaturecooled
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated to dryness
  7. customchromatographed on a column of silica gel which
  8. washis eluted with a mixture of chloroform and methanol (5, 10 and 20%)
  9. customThe combined pure fractions are evaporated to dryness
  10. customthe solid residue is crystallized from absolute ethanol
  11. customto provide the product

출처 및 근거

ORD 기록
ord-f67fd524b99c4fbb9b87bb40fbfeb07d
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05708171

연결된 노트

불러오는 중…