Ammonium Hydroxide → (+/-)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine

HRID 429847ノート

反応式

HRID 429847 の反応式
[CH3:1][CH:2]([CH3:19])[CH:3]([C:9]1[CH:14]=[CH:13][C:12]([NH:15]C(=O)C)=[CH:11][CH:10]=1)[N:4]1[CH:8]=[N:7][CH:6]=[N:5]1.[NH4+].[OH-]>Cl>[CH3:1][CH:2]([CH3:19])[CH:3]([C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=1)[N:4]1[CH:8]=[N:7][CH:6]=[N:5]1

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 9903273(+/-)-N-[4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]phenyl]acetamide

生成物 1

HCID 10900053(+/-)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine収率 75.4%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
60 °C

実験手順

A mixture of (±)-N-[4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]phenyl]acetamide (0.095 mol) in HCl (3N) (250 ml) was stirred and heated at 60° C. for 5 hours. The mixture was cooled, poured into ice, basified with concentrated NH4OH and extracted with CH2Cl2. The organic layer was dried, filtered off and evaporated. The residue was crystallized from 2-propanone/(C2H5)2O and filtered off, yielding 15.5 g (75%) of (±)-4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-benzenamine (interm. 2; mp. 117.8° C.).

後処理

  1. temperatureThe mixture was cooled
  2. additionpoured into ice
  3. extractionextracted with CH2Cl2
  4. customThe organic layer was dried
  5. filtrationfiltered off
  6. customevaporated
  7. customThe residue was crystallized from 2-propanone/(C2H5)2O
  8. filtrationfiltered off

出典と根拠

ORDレコード
ord-ce113939538a44fd88773132f7789e9a
出典データセット
uspto-grants-2001_11
特許番号
US06319939B1

反応ノート

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