ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Pyridine → 2-(2H-Benzo[D][1,2,3]triazol-2-YL)ethanamine

HRID 2257813
ノート
印刷プレビュー

反応式

HRID 2257813 の反応式
[N:1]1[N:2]([CH2:10][CH2:11]O)[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[N:13]1C=CC=CC=1.S(OS(C(F)(F)F)(=O)=O)(C(F)(F)F)(=O)=O>C(OCC)C>[N:1]1[N:2]([CH2:10][CH2:11][NH2:13])[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 817804HCID 817804、化合物

生成物 1

HCID 104872022-(2H-Benzo[D][1,2,3]triazol-2-YL)ethanamine収率 44,791.699%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
-50 °C

実験手順

4.70 g of the 2-(2-benzotriazolyl)ethanol (28.8 mmol) was dissolved in 200 ml diethyl ether and 2.28 g pyridine (28.8 mmol) was added. The mixture was cooled to -50° C., and 8.18 g triflic anhydride (29 mmol) was added. The mixture was removed from the cooling bath, and was allowed to reach room temperature. The mixture was filtered under dry conditions and added to a cold -40° C. solution of ca 150 ml ammonia in 50 ml diethyl ether. This mixture was allowed to reach room temperature, and ether was removed. 50 ml 2M HCl was added, and this mixture was washed with methylene chloride. The aqueous phase was made basic by addition of 50 ml 25% sodium hydroxide and extracted with 3×25 ml methylene chloride. Evaporation of the solvent gave 2.10 g 2-(2-benzotriazolyl)ethylamine (12.9 mol). This amine was used in the next step without further purification.

後処理

  1. customThe mixture was removed from the cooling bath
  2. customto reach room temperature
  3. filtrationThe mixture was filtered under dry conditions
  4. additionadded to a cold -40° C. solution of ca 150 ml ammonia in 50 ml diethyl ether
  5. customto reach room temperature
  6. customether was removed
  7. addition50 ml 2M HCl was added
  8. washthis mixture was washed with methylene chloride
  9. additionThe aqueous phase was made basic by addition of 50 ml 25% sodium hydroxide
  10. extractionextracted with 3×25 ml methylene chloride
  11. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-e8e6eb5c25084d7d942fdf6b2652be34
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05658907

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート