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Iodoethane → HCID 69358200, 화합물

HRID 852636
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HRID 852636 반응식
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])[CH:7]=[C:6]([OH:16])[CH:5]=1.C([O-])([O-])=O.[K+].[K+].[CH2:24](I)[CH3:25]>CN(C=O)C.Cl>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])[CH:7]=[C:6]([O:16][CH2:24][CH3:25])[CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 22252977Methyl 3-hydroxy-5-(2-oxopyrrolidin-1-yl)benzoate

생성물 1

HCID 69358200HCID 69358200, 화합물수율 95%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

To 3-hydroxy-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (D37) (0.80 g, 3.4 mmol, 1 equiv) dissolved in DMF (10 ml) was added K2CO3 (0.94 g, 6.8 mmol, 2 equiv) and ethyl iodide (1.1 g, 6.8 mmol, 2 equiv). The resulting mixture was heated at 50° C. for 4 h, cooled to room temperature, diluted with 2N aqueous HCl solution (50 ml) and extracted with Et2O (50 ml). The organic phase was then washed with water (50 ml), dried over MgSO4 and concentrated in vacuo to give of 3-ethoxy-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (B11) (0.85 g, 95%) as a brown oil which slowly solidified to a tan solid.

후처리

  1. temperaturecooled to room temperature
  2. extractionextracted with Et2O (50 ml)
  3. washThe organic phase was then washed with water (50 ml)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-93dc4936bfc2454481df94cb20dbf2db
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253198B2

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