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

HRID 1613120

反応式

HRID 1613120 の反応式
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

参加物

6

反応物 4

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 31374DimethylacetamideHCID 178478652HCID 178478652、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-015a1ffb1aa041e18734c98a8082ceec
出典データセット
uspto-grants-1993_03
特許番号
US05192647

関連ノート

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