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Methacrylic Acid → HCID 19063423, 화합물

HRID 1488876
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HRID 1488876 반응식
CC(C)([O-])C.[K+].[C:7]([OH:12])(=[O:11])[C:8]([CH3:10])=[CH2:9].[C:13](=[O:21])([O:17][CH2:18][CH2:19]Cl)[O:14][CH2:15][CH3:16].C1OCCOCCOCCOCCOCCOC1>CN(C=O)C>[C:13](=[O:21])([O:17][CH:18]([O:11][C:7](=[O:12])[C:8]([CH3:10])=[CH2:9])[CH3:19])[O:14][CH2:15][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4093Methacrylic AcidHCID 2855718-Crown-6HCID 12238111ethyl (chloroethoxy)formateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 19063423HCID 19063423, 화합물수율 38%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium tert. butoxide (3.70 g, 0.033 mol ) was added to a solution of methacrylic acid (2.84 g, 0.033 mol) in DMF (100 ml). Ethyl chloroethyl carbonate (5.08 g, 0.033 mol) from Example 1q(i) above was added to the resulting suspension. 18-crown-6 (0.61 g, 2.3 mmol) was then added and the reaction mixture was left with stirring at room temperature for 3 days. The reaction mixture was filtered and the solvent was removed under reduced pressure. The residue was dissolved in chloroform (100 ml) and washed with saturated aqueous sodium hydrogen carbonate (50 ml) and water (50 ml). The organic phase was dried (MgSO4) and the solvent removed under reduced pressure. Flash chromatography gave 2.50 g (38%) of the title product. (Adjusted for recovered starting material the yield was 75%).

후처리

  1. waitthe reaction mixture was left
  2. filtrationThe reaction mixture was filtered
  3. customthe solvent was removed under reduced pressure
  4. dissolutionThe residue was dissolved in chloroform (100 ml)
  5. washwashed with saturated aqueous sodium hydrogen carbonate (50 ml) and water (50 ml)
  6. dry with materialThe organic phase was dried (MgSO4)
  7. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-7291275d4ce5451e93188577d43d48e0
출처 데이터셋
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05676925

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