Water → 31309-58-7

HRID 1906201ノート

反応式

HRID 1906201 の反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[CH3:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:9][N:10]([CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

6

反応物 4

HCID 962WaterHCID 7515N-MethylanilineHCID 11430Potassium CarbonateHCID 23393Picolyl chloride

生成物 1

HCID 1421163431309-58-7収率 50.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A mixture of 2-chloromethylpyridine (50 g), N-methylaniline (42 g), and potassium carbonate (120 g) in N,N-dimethylformamide (200 ml) was stirred for 4 hours at 120° C. The reaction mixture was cooled to room temperature, added to water (1 l), and extracted with ether. The ether extract was washed with water and then treated with activated carbon. After drying over magnesium sulfate, the ether extract was filtered and concentrated. The residue was crystallized from isopropyl alcohol to give N-methyl-N-(2-pyridylmethyl)aniline (39 g).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionextracted with ether
  3. extractionThe ether extract
  4. washwas washed with water
  5. additiontreated with activated carbon
  6. dry with materialAfter drying over magnesium sulfate
  7. extractionthe ether extract
  8. filtrationwas filtered
  9. concentrationconcentrated
  10. customThe residue was crystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-bbfa271d7f044856993083f5cf71c13e
出典データセット
uspto-grants-1987_03
特許番号
US04650804

反応ノート

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