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

HRID 1717330노트

반응식

HRID 1717330 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 866298054-azido-3-ethoxy-N-ethylbenzamide수율 85%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-0c80758f338a4dcb9963d20409d2dab9
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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