Piperidine → HCID 21490881、化合物

HRID 1973897ノート

反応式

HRID 1973897 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5](Cl)[N:4]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1>>[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH2:10][CH2:11][CH2:12][CH3:13])=[C:5]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)[N:4]=1

参加物

3

反応物 2

HCID 8082PiperidineHCID 21490887HCID 21490887、化合物

生成物 1

HCID 21490881HCID 21490881、化合物

実験手順

46.8 g (0.2 mol) of 2-hydroxymethyl-4,6-dichloro-5-n-butyl-pyridine dissolved in 425 g (5 mols) of piperidine are heated for 20 hours at 190° in a bomb tube. The reaction mixture is then evaporated and the piperidine which still adheres is distilled off by means of toluene. The residue is rendered alkaline with 2 N sodium carbonate solution and the mixture is extracted with ether. The ether phases are combined, dried over sodium sulphate, filtered and evaporated. Fractional distillation of the residue in a high vacuum yields 2-hydroxymethyl-4-chloro-5-n-butyl-6-piperidino-pyridine of the formula ##STR17## and of boiling point 147°-152° (0.25 mm Hg).

後処理

  1. temperatureare heated for 20 hours at 190° in a bomb tube
  2. customThe reaction mixture is then evaporated
  3. distillationthe piperidine which still adheres is distilled off by means of toluene
  4. extractionthe mixture is extracted with ether
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated
  8. distillationFractional distillation of the residue in a high vacuum

出典と根拠

ORDレコード
ord-8dec4c71afc64d7ba1dff8a8ffe43259
出典データセット
uspto-grants-1976_12
特許番号
US03998955

反応ノート

読み込み中…