Pyridine → HCID 58446806、化合物

HRID 1958343ノート

反応式

HRID 1958343 の反応式
Br.[NH2:2][C:3]1[CH:8]=[CH:7][N:6]2[CH:9]=[C:10]([C:12]3[CH:13]=[C:14]([OH:18])[CH:15]=[CH:16][CH:17]=3)[N:11]=[C:5]2[N:4]=1.[C:19](OC(=O)C)(=[O:21])[CH3:20].N1C=CC=CC=1.C([O-])(O)=O.[Na+]>O>[NH2:2][C:3]1[CH:8]=[CH:7][N:6]2[CH:9]=[C:10]([C:12]3[CH:13]=[C:14]([O:18][C:19](=[O:21])[CH3:20])[CH:15]=[CH:16][CH:17]=3)[N:11]=[C:5]2[N:4]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 673879503-(7-Aminoimidazo[1,2-a]pyrimidin-2-yl)phenol hydrobromide

生成物 1

HCID 58446806HCID 58446806、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

To a microwave vial were added 3-(7-aminoimidazo[1,2-a]pyrimidin-2-yl)phenol hydrobromide (500 mg, 1.63 mmol), acetic anhydride (199 mg, 185 μA, 1.95 mmol) and pyridine (5.00 ml). The vial was capped and heated in the microwave at 120° C. for 15 min. H2O was added to the reaction mixture and the pH was installed around 7-8 by addition of 10% NaHCO3 aq. solution. The product was extracted with CH2Cl2, then the solvent was partially evaporated and the formed solid was collected and purified by flash chromatography (SiO2 cartridge; eluent: CH2Cl2/MeOH/NH3aq. 140:10:1). White solid (207 mg, 45%).

後処理

  1. customThe vial was capped
  2. extractionThe product was extracted with CH2Cl2
  3. customthe solvent was partially evaporated
  4. customthe formed solid was collected
  5. custompurified by flash chromatography (SiO2 cartridge; eluent: CH2Cl2/MeOH/NH3aq. 140:10:1)

出典と根拠

ORDレコード
ord-23c58876ba114e87b7ab7047b3753644
出典データセット
uspto-grants-2013_04
特許番号
US08410117B2

反応ノート

読み込み中…