Sodium Bicarbonate → 2-Chloro-5H-pyrrolo[3,2-d]pyrimidine

HRID 1803907

反応式

HRID 1803907 の反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[NH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.C(=O)([O-])O.[Na+]>C(O)C.[Pd]>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[NH:10][CH:9]=[CH:8][C:6]=2[N:7]=1

参加物

5

反応物 2

HCID 516892Sodium BicarbonateHCID 53750532,4-Dichloro-5H-pyrrolo[3,2-d]pyrimidine

生成物 1

HCID 457899862-Chloro-5H-pyrrolo[3,2-d]pyrimidine収率 61%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a solution of 2,4-dichloro-5H-pyrrolo[3,2-d]pyrimidine (6.6 g, 35.3 mmol) in ethanol (200 mL) was added sodium hydrogen carbonate (2.96 g) and Palladium on carbon (10%, 0.66 g). The mixture was stirred under an atmosphere of hydrogen at room temperature for 3 h. The mixture was filtered then filtrate absorbed onto silica gel. Flash chromatography, eluting with chloroform/methanol 4/1, afforded 2-chloro-5H-pyrrolo[3,2-d]pyrimidine (3.3 g, 61%). Also recovered from the column was 5H-pyrrolo[3,2-d]pyrimidine (1.5 g)

後処理

  1. filtrationThe mixture was filtered
  2. customfiltrate absorbed onto silica gel
  3. washFlash chromatography, eluting with chloroform/methanol 4/1

出典と根拠

ORDレコード
ord-e94e584325ec447c93a8608260ad190a
出典データセット
uspto-grants-2013_01
特許番号
US08354408B2

関連ノート

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