Hydrochloric Acid → 4-Aminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine

HRID 1613291ノート

反応式

HRID 1613291 の反応式
C([NH:4][CH2:5][C:6]1[CH2:7][CH2:8][N:9]([CH2:12][CH3:13])[CH2:10][CH:11]=1)(=O)C.[OH-].[Na+].Cl>CO>[NH2:4][CH2:5][C:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH3:13])[CH2:8][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 150234574-Acetylaminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine

生成物 1

HCID 150234584-Aminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine収率 92.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 4-acetylaminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine (20.0 g) and 6N aqueous solution of sodium hydroxide (73 ml) in methanol (150 ml) was refluxed for 40 hours. The solution was acidified with concentrated hydrochloric acid under ice cooling and evaporated in vacuo. To the residue was added ethanol (400 ml) and the mixture was refluxed for an hour. The resulting precipitates were filtered off and the filtrate was evaporated in vacuo. The residue was treated with Amberlite IRA-910 (trademark: Rohm & Haas Co.) and purified by vacuum distillation to give 4-aminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine (14.25 g).

後処理

  1. customevaporated in vacuo
  2. additionTo the residue was added ethanol (400 ml)
  3. temperaturethe mixture was refluxed for an hour
  4. customThe resulting precipitates
  5. filtrationwere filtered off
  6. customthe filtrate was evaporated in vacuo
  7. additionThe residue was treated with Amberlite IRA-910 (trademark: Rohm & Haas Co.)
  8. distillationpurified by vacuum distillation

出典と根拠

ORDレコード
ord-d45ca91d23ab4553a69d6670f6cb5044
出典データセット
uspto-grants-1993_03
特許番号
US05192779

反応ノート

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