Ethylene Glycol → 2-Amino-4,6-dimethylpyridine-3-carbaldehyde

HRID 1730647

반응식

HRID 1730647 반응식
C([O-])(C)C.[NH2:5][C:6]1[N:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[C:7]=1[C:8](NNS(C1C=CC=CC=1)(=O)=O)=[O:9].C(O)CO.C(=O)([O-])[O-].[Na+].[Na+].O>C(Cl)(Cl)Cl>[NH2:5][C:6]1[N:24]=[C:23]([CH3:25])[CH:22]=[C:21]([CH3:26])[C:7]=1[CH:8]=[O:9]

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 962WaterHCID 10340Sodium CarbonateHCID 86734206N1-(2-amino-4,6-dimethylnicotinoyl)-N2-benzenesulfonyl hydrazine isopropanolate

생성물 1

HCID 123666092-Amino-4,6-dimethylpyridine-3-carbaldehyde

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
160 °C

실험 절차

N1 -(2-amino-4,6-dimethylnicotinoyl)-N2 -benzenesulfonyl hydrazine isopropanolate (62.0 g., 0.163 mole) is divided into two portions. To each portion, ethylene glycol (300 ml.) is added and the mixture heated to 160° C. prior to the addition of anhydrous sodium carbonate (30 g.) in one portion with vigorous stirring. The mixture is allowed to cool and then is poured into water. The two runs are combined and the product isolated by extraction with chloroform. Following recrystallization from carbon tetrachloride the product melts at 152°-158° C. Further recrystallization from the same solvent raises the melting point to 162°-166° C.

후처리

  1. temperatureto cool
  2. customrecrystallization from carbon tetrachloride the product melts at 152°-158° C
  3. customFurther recrystallization from the same solvent
  4. temperatureraises the melting point to 162°-166° C.

출처 및 근거

ORD 기록
ord-a5fc3901f5e14b709cbce82790499b96
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993656

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