Sulfuric Acid → 5-acetylamino-1-(o-chlorobenzyl)-1H-1,2,3-triazole-4-carboxamide

HRID 414090노트

반응식

HRID 414090 반응식
[NH2:1][C:2]1[N:6]([CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[Cl:14])[N:5]=[N:4][C:3]=1[C:15]([NH2:17])=[O:16].[CH3:18][C:19](OC(C)=O)=[O:20].S(=O)(=O)(O)O>C(O)C>[C:19]([NH:1][C:2]1[N:6]([CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[Cl:14])[N:5]=[N:4][C:3]=1[C:15]([NH2:17])=[O:16])(=[O:20])[CH3:18]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 28153125-amino-1-[(2-chlorophenyl)methyl]-1H-1,2,3-triazole-4-carboxamide

생성물 1

HCID 212825985-acetylamino-1-(o-chlorobenzyl)-1H-1,2,3-triazole-4-carboxamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

10,1 g of 5-amino-1-(o-chlorobenzyl)-1H-triazole-4-carboxamide are added, portionwise with stirring, to a mixture of 30,7 g of acetanhydride and 0,1 ml of sulphuric acid and heated to 60° . Stirring is continued for additional 30 minutes at 60° to 70° , the reaction mixture is poored into 250 ml of ethanol, heated to reflux for 30 minutes and evaporated in vacuo to dryness. The residue is triturated with 250 ml of ethyl acetate, the crystalline precipitate is collected and re-crystallised from ethyl acetate yielding 5-acetylamino-1-(o-chlorobenzyl)-1H-1,2,3-triazole-4-carboxamide of m.p. 181°-183°.

후처리

  1. temperatureheated to 60°
  2. temperatureheated
  3. temperatureto reflux for 30 minutes
  4. customevaporated in vacuo to dryness
  5. customThe residue is triturated with 250 ml of ethyl acetate
  6. customthe crystalline precipitate is collected
  7. customre-crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-72fec188baa94a90bba1a455e65c2b69
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04789680

반응 노트

불러오는 중…