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Methanol → 5-amino-8-cyclopropyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 2386676
ノート
印刷プレビュー

反応式

HRID 2386676 の反応式
[N:1]([C:4]1[C:13]2[CH:12]=[N:11][C:10]([S:14][CH3:15])=[N:9][C:8]=2[N:7]([CH:16]2[CH2:18][CH2:17]2)[C:6](=[O:19])[CH:5]=1)=[N+]=[N-].C(Cl)Cl.CO>C(O)(=O)C.[OH-].[OH-].[Pd+2]>[NH2:1][C:4]1[C:13]2[CH:12]=[N:11][C:10]([S:14][CH3:15])=[N:9][C:8]=2[N:7]([CH:16]2[CH2:18][CH2:17]2)[C:6](=[O:19])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 6344DichloromethaneHCID 57929482HCID 57929482、化合物

生成物 1

HCID 579294555-amino-8-cyclopropyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one収率 125.2%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 176Acetic Acid
溶媒

実験手順

Palladium hydroxide on carbon (10% wt., 150 mg) was added to a solution of 5-azido-8-cyclopropyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one (1.5 g) in glacial acetic acid (80 mL) and the resulting mixture was stirred under H2 (balloon pressure) for 2 h. A mixture of DCM and MeOH (80/20, 100 mL) was added and the resulting mixture was filtered over a CELITE™ pad and the filter cake was washed with a mixture of DCM and MeOH (80/20, 500 mL). The filtrate was concentrated under reduced pressure to give 1.7 g 5-amino-8-cyclopropyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one as a green solid without further purifications. MS=248.9 [M+H]+.

後処理

  1. additionwas added
  2. filtrationthe resulting mixture was filtered over a CELITE™ pad
  3. washthe filter cake was washed with a mixture of DCM and MeOH (80/20, 500 mL)
  4. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b9d68a57545649688edaace3a351311a
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268840B2

反応ノート

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