Diethylamine → HCID 20321213、化合物

HRID 866413ノート

反応式

HRID 866413 の反応式
[CH3:1][C:2]1[N:3]=[C:4]([N+:11]([O-:13])=[O:12])[CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=O.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C(Cl)(Cl)Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:7](=[O:9])[C:6]1[CH:10]=[C:2]([CH3:1])[N:3]=[C:4]([N+:11]([O-:13])=[O:12])[CH:5]=1)[CH3:15]

参加物

5

反応物 3

HCID 8021DiethylamineHCID 14812Phosphorus oxide (P4O10)HCID 124040282-Methyl-6-nitropyridine-4-carboxylic acid

生成物 1

HCID 20321213HCID 20321213、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a mixture of 1.0 g. of 6-methyl-2-nitroisonicotinic acid, 20 ml. of chloroform and 3 ml. of diethylamine was added 7.0 g. of phosphorus pentoxide with stirring. The resulting mixture was refluxed for 1 hour. After cooling, the chloroform layer was separated and poured into 20 ml. of water. The resulting mixture was neutralized with sodium hydrogencarbonate and the chloroform layer was separated, dried over anhydrous sodium sulfate and the chloroform was distilled off in vacuo. The residual oil was gradually crystallized and then recrystallized from ethyl acetate-n-hexane to give 0.6 g. of the desired product.

後処理

  1. additionTo a mixture of 1.0 g
  2. temperatureThe resulting mixture was refluxed for 1 hour
  3. temperatureAfter cooling
  4. customthe chloroform layer was separated
  5. additionpoured into 20 ml
  6. customthe chloroform layer was separated
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationthe chloroform was distilled off in vacuo
  9. customThe residual oil was gradually crystallized
  10. customrecrystallized from ethyl acetate-n-hexane
  11. customto give 0.6 g

出典と根拠

ORDレコード
ord-3131f104a6e144bdbf284598435d6bbc
出典データセット
uspto-grants-1978_07
特許番号
US04098893

反応ノート

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