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Potassium Hydroxide → 5-Acetyl-2-(4-azidobutyl)-1,4-dihydro-6-methyl-4-(4-nitrophenyl)pyridine-3-carboxylic acid

HRID 964307
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HRID 964307 반응식
[C:1]([C:4]1[CH:5]([C:25]2[CH:30]=[CH:29][C:28]([N+:31]([O-:33])=[O:32])=[CH:27][CH:26]=2)[C:6]([C:18]([O:20]CCC#N)=[O:19])=[C:7]([CH2:11][CH2:12][CH2:13][CH2:14][N:15]=[N+:16]=[N-:17])[NH:8][C:9]=1[CH3:10])(=[O:3])[CH3:2].[OH-].[K+]>CC(C)=O>[C:1]([C:4]1[CH:5]([C:25]2[CH:30]=[CH:29][C:28]([N+:31]([O-:33])=[O:32])=[CH:27][CH:26]=2)[C:6]([C:18]([OH:20])=[O:19])=[C:7]([CH2:11][CH2:12][CH2:13][CH2:14][N:15]=[N+:16]=[N-:17])[NH:8][C:9]=1[CH3:10])(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 230040535-Acetyl-2-(4-azidobutyl)-3-(2-cyanoethoxy)carbonyl-1,4-dihydro-6-methyl-4-(4-nitrophenyl)pyridine

생성물 1

HCID 230041805-Acetyl-2-(4-azidobutyl)-1,4-dihydro-6-methyl-4-(4-nitrophenyl)pyridine-3-carboxylic acid수율 64.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 5-acetyl-2-(4-azidobutyl)-3-(2-cyanoethoxy)carbonyl-1,4-dihydro-6-methyl-4-(4-nitrophenyl)pyridine (1.05 g, 2.32 mmol) in 10 ml of acetone was treated with 20 ml of 1N aqueous KOH solution at 0° C. for 1 hr. The acetone was removed in vacuo and the aqueous layer was acidified to pH=3 by 2N hydrochloric acid, the resulting yellow precipitate was collected by filtration, washed with 10 ml of cold water and dried in vacuo to yield 0.60 g (60% yield) of 5-acetyl-2-(4-azidobutyl)-1,4-dihydro-6-methyl-4-(4-nitrophenyl)pyridine-3-carboxylic acid as a yellow powder.

후처리

  1. customThe acetone was removed in vacuo
  2. filtrationthe resulting yellow precipitate was collected by filtration
  3. washwashed with 10 ml of cold water
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-2458410b114a4e5382715834f407069d
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05767131

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