Sodium Hydroxide → CID 136342890

HRID 869481

反応式

HRID 869481 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 136342890CID 136342890収率 70%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

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]−.

後処理

  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

出典と根拠

ORDレコード
ord-156c90d4d22747109081027bf45a25b6
出典データセット
uspto-grants-2015_03
特許番号
US08969363B2

関連ノート

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