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

HRID 1730647

反応式

HRID 1730647 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
160 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-a5fc3901f5e14b709cbce82790499b96
出典データセット
uspto-grants-1976_11
特許番号
US03993656

関連ノート

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