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Iodoethane → HCID 68538880, 화합물

HRID 852542
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HRID 852542 반응식
C([O-])([O-])=O.[K+].[K+].I[CH2:8][CH3:9].[CH3:10][O:11][C:12](=[O:24])[C:13]1[CH:22]=[C:21]([OH:23])[CH:20]=[C:15]([C:16]([O:18][CH3:19])=[O:17])[CH:14]=1>CC(C)=O>[CH3:19][O:18][C:16](=[O:17])[C:15]1[CH:20]=[C:21]([O:23][CH2:8][CH3:9])[CH:22]=[C:13]([C:12]([O:11][CH3:10])=[O:24])[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 830651,3-Benzenedicarboxylic acid, 5-hydroxy-, 1,3-dimethyl ester

생성물 1

HCID 68538880HCID 68538880, 화합물수율 96.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

K2CO3 (31.6 g, 223 mmol, 2.23 equiv) and iodoethane (17.8 ml, 230 mmol, 2.3 equiv) were added to a solution of 5-hydroxy-isophthalic acid dimethyl ester (D42) (21 g, 100 mmol, 1 equiv) in acetone (500 ml) at room temperature. The resulting solution was refluxed for 16 h, then cooled to room temperature and concentrated in vacuo. The residue was partitioned between H2O and AcOEt. The aqueous phase was extracted with AcOEt and the combined organic layers were washed with 2N aqueous NaOH solution and brine, dried over MgSO4 and concentrated in vacuo to give 5-ethoxy-isophthalic acid dimethyl ester (D43) (23 g, 96%) as a white solid. RT=3.13 min

후처리

  1. temperatureThe resulting solution was refluxed for 16 h
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between H2O and AcOEt
  4. extractionThe aqueous phase was extracted with AcOEt
  5. washthe combined organic layers were washed with 2N aqueous NaOH solution and brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f3f407b290094123a34e68ec9fe9ea4a
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253198B2

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