Sodium Azide → 4-azido-3-ethoxy-N-ethylbenzamide

HRID 1717330ノート

反応式

HRID 1717330 の反応式
[NH2:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([NH:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=1[O:13][CH2:14][CH3:15].N([O-])=O.[Na+].[N-:20]=[N+:21]=[N-].[Na+]>Cl>[N:1]([C:2]1[CH:12]=[CH:11][C:5]([C:6]([NH:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=1[O:13][CH2:14][CH3:15])=[N+:20]=[N-:21]

参加物

5

反応物 3

HCID 33557Sodium AzideHCID 23668193Sodium NitriteHCID 633585494-amino-3-ethoxy-N-ethylbenzamide

生成物 1

HCID 866298054-azido-3-ethoxy-N-ethylbenzamide収率 85%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a solution of 4-amino-3-ethoxy-N-ethylbenzamide (0.53 g) obtained in Example 131c) in 0.2N hydrochloric acid (12.5 ml) was added 1M aqueous sodium nitrite solution (2.5 ml) under ice-cooling, and the mixture was stirred for 2 hr. To the obtained reaction mixture was added an aqueous solution (5 ml) of sodium azide (0.17 g) under ice-cooling, and the mixture was stirred for 30 min. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a yellow oil (0.50 g, 85%).

後処理

  1. temperaturecooling
  2. customTo the obtained reaction mixture
  3. temperaturecooling
  4. stirringthe mixture was stirred for 30 min
  5. extractionThe reaction mixture was extracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0c80758f338a4dcb9963d20409d2dab9
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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