Methyl iodide → HCID 13692943, 화합물

HRID 255883

반응식

HRID 255883 반응식
OC1[CH:10]=[CH:9][CH:8]=[C:7]2C=1[CH2:4][CH2:5][C:6]2=[O:11].[H-].[Na+].[CH3:14]I.[CH2:16]1[CH2:20][O:19][CH2:18][CH2:17]1>>[CH3:14][C:5]1([CH3:4])[CH2:17][C:16]2[C:7](=[CH:8][CH:9]=[CH:10][C:20]=2[O:19][CH3:18])[C:6]1=[O:11]

참가 물질

5

반응물 4

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 5905474-Hydroxy-1-indanone

생성물 1

HCID 13692943HCID 13692943, 화합물

실험 절차

4-Hydroxy-indanone (25 g) is added portionwise to a stirred suspension of sodium hydride (40.1 g, 60% in mineral oil) and methyl iodide (62.4 g) in anhydrous THF (990 ml) under nitrogen and the mixture is stirred at RT overnight. The reaction mixture is quenched with H2O, washed with diethyl ether and the etheral layer is washed with 10% aq. NaHSO3 and H2O, dried, filtered, and evaporated. The residue is chromatographed (silica gel; eluent=hexane/EtOAC) affording the desired product as a solid.

후처리

  1. customThe reaction mixture is quenched with H2O
  2. washwashed with diethyl ether
  3. washthe etheral layer is washed with 10% aq. NaHSO3 and H2O
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is chromatographed (silica gel; eluent=hexane/EtOAC)

출처 및 근거

ORD 기록
ord-bb2a6ed572d8406ab7a288aafce2c017
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04699906

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