Triethylamine → Phenyl 1H-benzo[d][1,2,3]triazol-5-ylcarbamate

HRID 1613120

반응식

HRID 1613120 반응식
Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1.CC(N(C)C)=O.C(N(CC)CC)C.[C:26](Cl)(=[O:34])[O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>N1C=CC=CC=1>[O:27]([C:26]([NH:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1)=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 31374DimethylacetamideHCID 178478652HCID 178478652, 화합물

생성물 1

HCID 178521835Phenyl 1H-benzo[d][1,2,3]triazol-5-ylcarbamate수율 88.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
5 °C

실험 절차

To 62.1 g of 5-aminobenzotriazole dihydrochloride was added 500 ml of dimethylacetamide, and 83,7 ml of triethylamine was added dropwise thereto while being cooled in an ice bath. To the mixture was further added dropwise 21.0 ml of pyridine, and 42.3 g of phenyl chlorocarbonate was then added dropwise thereto while maintaining the system at 5° C. or lower, followed by stirring at room temperature for 2 hours. After the reaction, the reaction mixture was poured into 2 (of ice-water for crystallization, followed by filtration to obtain 60.8 g of 5-phenoxycarbonylaminobenzotriazole.

후처리

  1. additionwas added dropwise
  2. temperaturewhile being cooled in an ice bath
  3. additionwas then added dropwise
  4. customAfter the reaction
  5. customfor crystallization
  6. filtrationfollowed by filtration

출처 및 근거

ORD 기록
ord-015a1ffb1aa041e18734c98a8082ceec
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05192647

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