Ethyl Bromide → HCID 58208009, 화합물

HRID 2197569노트

반응식

HRID 2197569 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 58208009HCID 58208009, 화합물수율 50%

시약·촉매·용매 2

HCID 180Acetone용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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%

출처 및 근거

ORD 기록
ord-706ac94243fa4842b64e196700aaa8e1
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338604B2

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