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Sodium Bicarbonate → 3-Methylspiro(indene-1,4'-piperidine)

HRID 1027137
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HRID 1027137 반응식
[CH3:1][C:2]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6][CH2:5]2)[CH:3]=1.C(=O)([O-])O.[Na+]>O1CCOCC1.Cl>[CH3:1][C:2]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:4]2([CH2:5][CH2:6][NH:7][CH2:8][CH2:9]2)[CH:3]=1
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 86646304HCID 86646304, 화합물

생성물 1

HCID 670830823-Methylspiro(indene-1,4'-piperidine)수율 94%

시약·촉매·용매 1

HCID 204431481,4-Dioxane hydrochloride용매

실험 절차

tert-Butyl 3-methylspiro[inden-1,4′-piperidine]-1′-carboxylate (0.155 g, 0.518 mmol) obtained in step 3 was dissolved in 4 mol/L hydrogen chloride-1,4-dioxane (2 mL), and the mixture was stirred at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the obtained residue, and the mixture was suction-filtered to give white crystals. Saturated aqueous sodium hydrogen carbonate solution was added to the white crystals, and the mixture was extracted with ethyl acetate. The combined organic layers were dried over magnesium sulfate, and concentrated under reduced pressure to give the title compound (0.097 g, 94%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
  2. additionwas added to the obtained residue
  3. filtrationthe mixture was suction-filtered
  4. customto give white crystals
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe combined organic layers were dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-146112c8e89247d5ba426035fa8e169b
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729264B2

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