Histamine → HCID 178526685、化合物

HRID 744048

反応式

HRID 744048 の反応式
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

参加物

4

反応物 2

HCID 774HistamineHCID 783082-Chloro-5-nitropyridine

生成物 1

HCID 178526685HCID 178526685、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d9177694b10946c99c1516e8b26713bf
出典データセット
uspto-grants-1996_09
特許番号
US05559113

関連ノート

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