Ethylene Glycol → Acetamide, N-(6-amino-5-formyl-2,4-dimethyl-3-pyridinyl)-

HRID 1730645노트

반응식

HRID 1730645 반응식
C(O)CO.[NH2:5][C:6]1[N:24]=[C:23]([CH3:25])[C:22]([NH:26][C:27](=[O:29])[CH3:28])=[C:21]([CH3:30])[C:7]=1[C:8](NNS(C1C=CC=CC=1)(=O)=O)=[O:9].C(=O)([O-])[O-].[Na+].[Na+].O>C(Cl)Cl>[NH2:5][C:6]1[N:24]=[C:23]([CH3:25])[C:22]([NH:26][C:27](=[O:29])[CH3:28])=[C:21]([CH3:30])[C:7]=1[CH:8]=[O:9]

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 962WaterHCID 10340Sodium CarbonateHCID 12297945HCID 12297945, 화합물

생성물 1

HCID 12297946Acetamide, N-(6-amino-5-formyl-2,4-dimethyl-3-pyridinyl)-

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
160 °C

실험 절차

Ethylene glycol (80 ml.) is heated in an oil-bath at 170° C. until the internal temperature reaches 160° C. N1 -(2-amino-5-acetamido-4,6-dimethylnicotinoyl)-N2 -benzenesulfonyl hydrazine (8.0 g., 21.2 mmole) is added and the mixture stirred until the internal temperature returns to 160° C. Anhydrous sodium carbonate (5.6 g.) is added in one portion, heating is continued for 30 seconds and the reaction mixture cooled rapidly and poured into water (320 ml.). The product is isolated by continuous extraction with methylene chloride for about 24 hours to give 2.90 g. (66%) of crude product. Following purification by crystallization from ethanol the pure product melts at 270°-275° C. (dec.) with rapid heating.

후처리

  1. customreaches 160° C
  2. temperatureheating
  3. temperaturethe reaction mixture cooled rapidly
  4. customto give 2.90 g
  5. custompurification
  6. customby crystallization from ethanol the pure product melts at 270°-275° C. (dec.) with rapid heating

출처 및 근거

ORD 기록
ord-410dff877ec44d2d80c2875c688a5daf
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993656

반응 노트

불러오는 중…