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

HRID 382753
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HRID 382753 반응식
[N:1]([CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[NH:9][C:10]([CH3:34])=[C:11]([C:30]([O:32][CH3:33])=[O:31])[CH:12]([C:21]2[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[CH:23][CH:22]=2)[C:13]=1[C:14]([O:16]CCC#N)=[O:15])=[N+:2]=[N-:3].[OH-].[K+]>CC(C)=O>[N:1]([CH2:4][CH2:5][CH2:6][CH2:7][C:8]1[NH:9][C:10]([CH3:34])=[C:11]([C:30]([O:32][CH3:33])=[O:31])[CH:12]([C:21]2[CH:22]=[CH:23][C:24]([N+:27]([O-:29])=[O:28])=[CH:25][CH:26]=2)[C:13]=1[C:14]([OH:16])=[O:15])=[N+:2]=[N-:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 865866352-(4-Azidobutyl)-3-(2-cyanoethoxy) carbonyl-1,4-dihydro-5-methoxycarbonyl-6-methyl-4-(4-nitrophenyl)pyridine

생성물 1

HCID 183607782-(4-Azidobutyl)-1,4-dihydro-5-methoxycarbonyl-6-methyl-4-(4-nitrophenyl)pyridine-3-carboxylic acid수율 61.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 2-(4-azidobutyl)-3-(2-cyanoethoxy)carbonyl-1,4-dihydro-5-methoxycarbonyl-6-methyl-4-(4-nitrophenyl)pyridine (1.38 g,. 2.95 mmol) in 10 ml acetone was treated with 15 ml 1N 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 750 mg (61% yield) of 2-(4-azidobutyl)-1,4-dihydro-5-methoxycarbonyl-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-b333439e425f4192b4e48204865a7cda
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310076B1

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