Sodium Carbonate → 5-Bromo-N4-(1-methylpiperidin-4-yl)pyridine-2,4-diamine

HRID 556843

反応式

HRID 556843 の反応式
[Br:1][C:2]1[C:3]([NH:15][CH:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)=[CH:4][C:5]([NH:8]C(=O)C(C)(C)C)=[N:6][CH:7]=1.C([O-])([O-])=O.[Na+].[Na+]>Cl>[Br:1][C:2]1[C:3]([NH:15][CH:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)=[CH:4][C:5]([NH2:8])=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 59613507N-(5-Bromo-4-(1-methylpiperidin-4-ylamino)pyridin-2-yl)pivalamide

生成物 1

HCID 596135485-Bromo-N4-(1-methylpiperidin-4-yl)pyridine-2,4-diamine収率 71.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of N-(5-bromo-4-(1-methylpiperidin-4-ylamino)pyridin-2-yl)pivalamide (0.526, 1.42 mmol) in 6M HCl (6 mL) was heated under microwave irradiation at 105° C. for 50 min. The solution was basified with Na2CO3 and extracted with ethyl acetate (3×20 mL). The crude mixture was purified by flash chromatography on silica, eluting with methanol and dichloromethane (1/9), to give the title compound as a colourless solid (0.288 g, 70%).

後処理

  1. extractionextracted with ethyl acetate (3×20 mL)
  2. customThe crude mixture was purified by flash chromatography on silica
  3. washeluting with methanol and dichloromethane (1/9)

出典と根拠

ORDレコード
ord-d1196fedb59c475eb22c200ad00be6ae
出典データセット
uspto-grants-2011_11
特許番号
US08058045B2

関連ノート

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