Hydrochloric Acid → Octyl 2-pyrazinecarboxylate

HRID 1440015ノート

反応式

HRID 1440015 の反応式
[CH2:1]([OH:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[N:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:16](O)=[O:17].Cl>C(Cl)Cl>[N:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:16]([O:9][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])=[O:17]

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 9571-OctanolHCID 10472-Pyrazinecarboxylic acid

生成物 1

HCID 465427Octyl 2-pyrazinecarboxylate収率 60.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A four-necked flask was charged with 100 g (0.768 mole) of 1-octanol and 10 g (0.081 mole) of pyrazinecarboxylic acid and while the internal temperature was maintained under stirring at 70°-80° C., 15 g (0.411 mole) of hydrogen chloride was introduced through a gas inlet tube over a period of 3 hours. Upon completion of the introduction of hydrogen chloride, the reaction mixture was cooled and 100 ml of methylene chloride was added. The mixture was transferred to a separatory funnel, in which it was washed with a small quantity of aqueous sodium carbonate solution. From the oil layer which separated, the methylene chloride was first distilled off and the residue was subjected to distillation under reduced pressure to give 11.5 g of octyl pyrazinecarboxylate. Yield: 60% (based on pyrazinecarboxylic acid)

後処理

  1. temperaturewas maintained
  2. customThe mixture was transferred to a separatory funnel, in which it
  3. washwas washed with a small quantity of aqueous sodium carbonate solution
  4. customFrom the oil layer which separated
  5. distillationthe methylene chloride was first distilled off
  6. distillationthe residue was subjected to distillation under reduced pressure

出典と根拠

ORDレコード
ord-43ec2ccfadbe4c6ab312224d2b92f934
出典データセット
uspto-grants-1996_03
特許番号
US05496949

反応ノート

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