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3-(4-Methyl-tetrahydro-pyran-4-yl)-acrylic acid ethyl ester → HCID 67528472, 화합물

HRID 1512177
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HRID 1512177 반응식
C([O:3][C:4](=[O:14])[CH:5]=[CH:6][C:7]1([CH3:13])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)C>CCO.[OH-].[Na+]>[CH3:13][C:7]1([CH:6]=[CH:5][C:4]([OH:14])=[O:3])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1
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참가 물질

4

반응물 1

HCID 675281893-(4-Methyl-tetrahydro-pyran-4-yl)-acrylic acid ethyl ester

생성물 1

HCID 67528472HCID 67528472, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

To a solution of 3-(4-methyl-tetrahydro-pyran-4-yl)-acrylic acid ethyl ester (396 mg, 2.00 mmol, prepared as in STEP A above) in EtOH (10 mL), 6N aqueous NaOH (1 mL) was added dropwise. The resulting mixture was stirred at room temperature over night. The resulting mixture was concentrated and the resulting residue was dissolved in 20 mL of water. The resulting solution was washed twice with diethyl ether (10 mL), and the aqueous layer was acidified with 6N HCl and extracted thrice with DCM (20 mL). The DCM layers were combined, dried over Na2SO4 and concentrated in vacuo to yield 3-(4-methyl-tetrahydro-pyran-4-yl)-acrylic acid, which was used in next step without further purification.

후처리

  1. concentrationThe resulting mixture was concentrated
  2. dissolutionthe resulting residue was dissolved in 20 mL of water
  3. washThe resulting solution was washed twice with diethyl ether (10 mL)
  4. extractionextracted thrice with DCM (20 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5c99a39bf5874d8890088b5beea8bb30
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217060B2

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