1-Methyl-5-nitro-1H-imidazole-2-carbaldehyde → HCID 54069604、化合物

HRID 1856193ノート

反応式

HRID 1856193 の反応式
[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[CH:10]=O.[CH3:12][C:13]1[S:14][CH:15]=[N:16][N:17]=1>C(O)(=O)C.C(OC(=O)C)(=O)C.[Cl-].[Zn+2].[Cl-]>[CH3:1][N:2]1[C:6]([N+:7]([O-:9])=[O:8])=[CH:5][N:4]=[C:3]1[CH:10]=[CH:12][C:13]1[S:14][CH:15]=[N:16][N:17]=1

参加物

6

反応物 2

HCID 784871-Methyl-5-nitro-1H-imidazole-2-carbaldehydeHCID 142788092-Methyl-1,3,4-thiadiazole

生成物 1

HCID 54069604HCID 54069604、化合物

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 176Acetic Acid溶媒2 回HCID 7918Acetic Anhydride溶媒2 回

実験手順

0.3 g of zinc chloride is added to 15.5 g of 1-methyl-5nitroimidazol-2-carboxaldehyde which has been dissolved in 100 ml of acetic acid and 50 ml of acetic anhydride and the whole is dripped into 10 g of 2-methyl-1,3,4-thiadiazole, which has been dissolved in a mixture of 100 ml of acetic acid and 50 ml of acetic anhydride, over a period of 5 hours at reflux temperature. After 24 hours the reaction mixture is freed of the solvent by evaporation and ether is added. After the reaction product has been washed with water it is recrystallized from xylene. 9.3 of product, corresponding to 39% of the theory, is obtained. The compound melts at 214° C.

後処理

  1. temperatureat reflux temperature
  2. customAfter 24 hours the reaction mixture is freed of the solvent by evaporation and ether
  3. additionis added
  4. washAfter the reaction product has been washed with water it
  5. customis recrystallized from xylene
  6. custom9.3 of product, corresponding to 39% of the theory, is obtained

出典と根拠

ORDレコード
ord-1333992633924f4fbb7846ada9aa6f90
出典データセット
uspto-grants-1980_08
特許番号
US04218460

反応ノート

読み込み中…