Histamine → HCID 178526685, 화합물

HRID 744048

반응식

HRID 744048 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-d9177694b10946c99c1516e8b26713bf
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05559113

연결된 노트

불러오는 중…