Ethyl Bromide → HCID 58208009、化合物

HRID 1958496ノート

反応式

HRID 1958496 の反応式
Cl.[Br:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6]2[N:7]([CH:9]=[CH:10][N:11]=2)[CH:8]=1.C([O-])([O-])=O.[Cs+].[Cs+].[CH2:19](Br)[CH3:20].CCOC(C)=O.CCCCCCC>CC(C)=O.CN(C=O)C>[Br:2][C:3]1[CH:4]=[C:5]([O:12][CH2:19][CH3:20])[C:6]2[N:7]([CH:9]=[CH:10][N:11]=2)[CH:8]=1

参加物

7

反応物 4

HCID 6332Ethyl BromideHCID 10796Cesium carbonateHCID 21899848Ethylacetate heptaneHCID 670075396-broMo-8-hydroxy-iMidazo[1,2-a] pyridine hydrochloride

生成物 1

HCID 58208009HCID 58208009、化合物収率 50%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6228Dimethylformamide溶媒

実験手順

6-Bromoimidazo[1,2-a]pyridin-8-ol hydrochloride (40 mg, 0.16 mmol) and Cs2CO3 (104 mg, 0.32 mmol) in acetone (0.64 mL) and DMF (0.2 mL) was added ethyl bromide (12 μL). The reaction was stirred for 48 h then the volatile solvents were removed and the residue then added water (0.8 mL). The resulting solids were stirred, filtered, and rinsed with water. The water filtrate was extracted with EtOAc and then combined with the solid crude products. The residue was purified via column chromatography (25% then 50% EtOAc/heptane) to afford the product (19 mg, 50% yield).

後処理

  1. customthe volatile solvents were removed
  2. stirringThe resulting solids were stirred
  3. filtrationfiltered
  4. washrinsed with water
  5. extractionThe water filtrate was extracted with EtOAc
  6. customThe residue was purified via column chromatography (25%

出典と根拠

ORDレコード
ord-0671a4b5f8784dc49cdbfbab7f045087
出典データセット
uspto-grants-2013_04
特許番号
US08410128B2

反応ノート

読み込み中…