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

HRID 1708353ノート

反応式

HRID 1708353 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1a1e6f22a662469d905037387cd9e2b0
出典データセット
uspto-grants-1994_10
特許番号
US05358939

反応ノート

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