Acetic Anhydride → N-{2-phenyl-2-[(1,2,4-triazol-1-yl)methyl]hexyl}acetamide

HRID 54909노트

반응식

HRID 54909 반응식
[C:1]1([C:7]([CH2:14][N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][NH2:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:20](OC(=O)C)(=[O:22])[CH3:21]>N1C=CC=CC=1>[C:1]1([C:7]([CH2:14][N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][NH:9][C:20](=[O:22])[CH3:21])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 199569622-Phenyl-2-[(1,2,4-triazol-1-yl)methyl]-1-hexylamine

생성물 1

HCID 15790295N-{2-phenyl-2-[(1,2,4-triazol-1-yl)methyl]hexyl}acetamide수율 89.3%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a 100 mL flask stirring under nitrogen was charged 2.58 g (0.010 mole) of 2-phenyl-2-[(1,2,4-triazol-1-yl)methyl]-1-hexylamine and 15 mL of acetic anhydride. To the mixture was added 1.5 mL of pyridine and the reaction was stirred at room temperature for 3 hours. After GLC indicated the reaction was complete, it was quenched with 20 mL of water and 100 mL of ether after the acetic anhydride and pyridine were removed under vacuum. The residue was dissolved in ether and washed with 2×50 mL water and 2×50 mL of saturated sodium bicarbonate. The organic phase was dried, concentrated and gave 2.68 g (89.3% yield) of a solid, melting point 112°-115° C.

후처리

  1. stirringthe reaction was stirred at room temperature for 3 hours
  2. customit was quenched with 20 mL of water and 100 mL of ether after the acetic anhydride and pyridine
  3. customwere removed under vacuum
  4. dissolutionThe residue was dissolved in ether
  5. washwashed with 2×50 mL water and 2×50 mL of saturated sodium bicarbonate
  6. customThe organic phase was dried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fc16da06b4e44ace8da0106784417fd8
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624916

반응 노트

불러오는 중…