Sodium Hydroxide → CID 136342890

HRID 869481

반응식

HRID 869481 반응식
[Cl:1][C:2]1[C:3]2[C:10]([CH:11]=O)=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1.Cl.[NH2:14][OH:15].[OH-].[Na+]>CCO.O>[Cl:1][C:2]1[C:3]2[C:10]([CH:11]=[N:14][OH:15])=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 567638284-Chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde

생성물 1

HCID 136342890CID 136342890수율 70%

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매

실험 절차

To a suspension of 4-chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde (1.17 g, 6.47 mmol, 1.0 eq) and hydroxylamine hydrochloride (0.54 g, 7.77 mmol, 1.2 eq) in EtOH (25 mL), aqueous NaOH solution (0.31 g, 7.77 mmol, 1.2 eq) in H2O (4 mL) was added dropwise. The resulting mixture was stirred at RT for 30 min and then was diluted with a sufficient amount of EtOH to allow stirring for additional 30 min. The solid was collected by filtration, rinsed with H2O and dried in vacuo to afford 4-chloro-7H-pyrrolo[2,3-d]pyrimidine-5-carbaldehyde oxime (0.89 g, 70% yield) as a mixture of isomers. ESI-MS m/z: 194.8 [M−H]−.

후처리

  1. additionwas added dropwise
  2. stirringto allow stirring for additional 30 min
  3. filtrationThe solid was collected by filtration
  4. washrinsed with H2O
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-156c90d4d22747109081027bf45a25b6
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969363B2

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