Methyl iodide → HCID 67304597, 화합물

HRID 1009010노트

반응식

HRID 1009010 반응식
[H-].[Na+].[CH3:3][C:4]1[CH:8]=[CH:7][O:6][C:5]=1[CH2:9][OH:10].I[CH3:12]>O1CCCC1>[CH3:12][O:10][CH2:9][C:5]1[O:6][CH:7]=[CH:8][C:4]=1[CH3:3]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 11194308(3-methyl-2-furyl)methanol

생성물 1

HCID 67304597HCID 67304597, 화합물수율 113.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under an inert atmosphere sodium hydride (0.25 g ˜60%, 6.2 mmol, 1.1 equiv.) was suspended in dry tetrahydrofuran. At 5° C. a solution of (3-methyl-furan-2-yl)-methanol (0.63 g, 5.6 mmol) in dry tetrahydrofuran was added dropwise. The mixture was stirred at room temp. for one hour, then iodomethane (0.9 g, 6.2 mmol, 1.1 equiv.) was added dropwise. The mixture was stirred overnight at room temp., quenched with diluted acid and extracted with diethyl ether. The combined, organic extracts were washed with brine, dried over magnesium sulfate dihydrate, filtered and concentrated under reduced pressure to give 0.8 g of the title compound as a light yellow oil. GC-MS (EI): M=126.

후처리

  1. stirringThe mixture was stirred overnight at room temp.
  2. customquenched
  3. additionwith diluted acid
  4. extractionextracted with diethyl ether
  5. washorganic extracts were washed with brine
  6. dry with materialdried over magnesium sulfate dihydrate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f0962129fe2648a0a9cc6bb8f2222eca
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973051B2

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