Diethylamine → HCID 20321213, 화합물

HRID 973061노트

반응식

HRID 973061 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 20321213HCID 20321213, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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 ever 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.

후처리

  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 ever 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

출처 및 근거

ORD 기록
ord-9509ca699a554d178bdc1d57ba2a9928
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04054663

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