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Methyl iodide → Methyl 2-methyl-2,3-dihydro-1H-indene-2-carboxylate

HRID 605520
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HRID 605520 반응식
[CH3:1][O:2][C:3]([CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)=[O:4].[Li+].[CH3:15][Si]([N-][Si](C)(C)C)(C)C.CI>C1COCC1>[CH3:1][O:2][C:3]([C:5]1([CH3:15])[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)=[O:4]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 2733832Lithium hexamethyldisilazaneHCID 9964238Methyl indane-2-carboxylate

생성물 1

HCID 57565328Methyl 2-methyl-2,3-dihydro-1H-indene-2-carboxylate수율 9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

Indane-2-carboxylic acid methyl ester (550 mg, 3.125 mmol) was dissolved in THF (20 mL). At −78° C. LiHMDS (1M solution in THF, 3.75 mL) was added into the reaction mixture. The solution was stirred for 15 min at −78° C., warmed to 0° C. for 15 min and then −78° C. for an additional 15 min. Methyl iodide (250 μL, 4.01 mmol) was then added into the reaction mixture followed by stirring at −78° C. for 15 min, room temperature for 30 min and then quenched with saturated ammonium chloride. The solution was then diluted with diethyl ether and washed with saturated sodium bicarbonate, brine, dried (MgSO4), filtered and concentrated. The crude mixture was then purified by silica gel flash column chromatography to afford 2-methyl-indan-2-carboxylic acid methyl ester (52 mg, 9%) as a white solid. 1H NMR (400 MHz, CDCl3) 7.16 (m, 4H), 3.72 (t, 3H), 3.48 (d, 2H), 2.81 (d, 2H), 1.36 (s, 3H).

후처리

  1. customAt −78° C
  2. temperaturewarmed to 0° C. for 15 min
  3. wait−78° C. for an additional 15 min
  4. stirringby stirring at −78° C. for 15 min, room temperature for 30 min
  5. customquenched with saturated ammonium chloride
  6. additionThe solution was then diluted with diethyl ether
  7. washwashed with saturated sodium bicarbonate, brine
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude mixture was then purified by silica gel flash column chromatography

출처 및 근거

ORD 기록
ord-5519ef80442043a7bcb8b3244d42f56f
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915253B2

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