1-Methyl-5-nitro-1H-imidazole-2-carbaldehyde → HCID 54069604, 화합물

HRID 1856193노트

반응식

HRID 1856193 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

HCID 54069604HCID 54069604, 화합물

시약·촉매·용매 3

HCID 3007855Zincchloride촉매HCID 176Acetic Acid용매2회HCID 7918Acetic Anhydride용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1333992633924f4fbb7846ada9aa6f90
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04218460

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