Formaldehyde → 2-Methyl-6-dimethylaminoethylpyrazine

HRID 981448

反応式

HRID 981448 の反応式
[CH3:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH3:8])[N:3]=1.Cl.[CH3:10][NH:11][CH3:12].[CH2:13]=O.[OH-].[Na+]>O>[CH3:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH2:8][CH2:10][N:11]([CH3:13])[CH3:12])[N:3]=1

参加物

6

反応物 4

HCID 712FormaldehydeHCID 79382,6-DimethylpyrazineHCID 10473Dimethylamine, hydrochlorideHCID 14798Sodium Hydroxide

生成物 1

HCID 544959662-Methyl-6-dimethylaminoethylpyrazine収率 32.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2,6-dimethylpyrazine (Pyrazine Specialities, Inc., Atlanta, Georgia, containing 2%, 2,5-isomer) (15.5 g) and dimethylamine hydrochloride (13.0 g) was heated until it began refluxing, and then formaldehyde (22.5 g as 38% aqueous solution) was added over a 30-min period. The resulting solution was refluxed for 2 hours. The solution was cooled to room temperature and diluted with water, made basic by the addition of 10% aqueous solution of sodium hydroxide, and extracted with chloroform. After removing the solvent, distillation of the residue gave 7.8 g of 2-methyl-6-dimethylaminoethylpyrazine with 5% of the 2,5-isomer (33% yield), 120°-126° C./12 mm Hg.

後処理

  1. temperaturewas heated until it
  2. temperaturebegan refluxing
  3. temperatureThe resulting solution was refluxed for 2 hours
  4. extractionextracted with chloroform
  5. customAfter removing
  6. distillationthe solvent, distillation of the residue

出典と根拠

ORDレコード
ord-78f54b2a0a8d4c83848f75557bac25cb
出典データセット
uspto-grants-1991_02
特許番号
US04992268

関連ノート

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