Hydroxyamine hydrochloride → 4-(3H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-one oxime

HRID 2243305노트

반응식

HRID 2243305 반응식
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[N:9]1[C:17]2[CH:16]=[CH:15][N:14]=[CH:13][C:12]=2[NH:11][C:10]=1[C:18]1[C:30]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23](=O)[C:22]=2[CH:21]=[CH:20][CH:19]=1>C(O)C.O>[N:9]1[C:17]2[CH:16]=[CH:15][N:14]=[CH:13][C:12]=2[NH:11][C:10]=1[C:18]1[C:30]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23](=[N:2][OH:3])[C:22]=2[CH:21]=[CH:20][CH:19]=1

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 533938014-(1h-Imidazo[4,5-C]pyridin-2-Yl)fluoren-9-One

생성물 1

HCID 1363601694-(3H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-one oxime수율 88.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

In a 500-ml three-necked flask, dissolve 20 g of 4-(3H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-one, obtained in Example 1, in 328 ml of ethanol, then add successively 14.02 g of hydroxylamine hydrochloride and 27.59 g of dry sodium acetate. After stirring overnight at room temperature, dilute with 328 ml of water. The precipitate that formed is drained, washed with water and dried in the stove at 500. In this way we obtain 18.6 g of equimolecular mixture of the Z and E oximes of 4-(3H-imidazo[4,5-c]pyridin-2-yl)-fluoren-9-one, in the form of a pale yellow powder, witH-NMR purity over 95%, with the following characteristics:

후처리

  1. customThe precipitate that formed
  2. washwashed with water
  3. customdried in the stove at 500

출처 및 근거

ORD 기록
ord-9a19354d52d3426fa9da2815eed9baf9
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674795B2

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