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Water → 1-Tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate

HRID 1510654
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HRID 1510654 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5]1([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1.C(OCC)(=O)C.O.[CH3:30][S:31](Cl)(=[O:33])=[O:32]>O1CCCC1.C(N(CC)CC)C>[CH3:30][S:31]([O:1][CH2:2][CH2:3][CH2:4][C:5]1([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)(=[O:33])=[O:32]
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참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 31297Methanesulfonyl chlorideHCID 578152391-Tert-butyl 4-ethyl 4-(3-hydroxypropyl)piperidine-1,4-dicarboxylate

생성물 1

HCID 578155261-Tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8471Triethylamine용매

실험 절차

To a solution of 1.7 g of 1-tert-butyl 4-ethyl 4-(3-hydroxypropyl)piperidine-1,4-dicarboxylate in 20 mL of tetrahydrofuran, 0.82 mL of triethylamine and 0.58 mL of methanesulfonyl chloride were added at 5° C., and the mixture was stirred at room temperature for 1 hour. Thereto were added ethyl acetate and water. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 1.9 g of 1-tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate as a colorless oily substance.

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with ethyl acetate
  3. washthe resultant solution was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-db97194df776427dad5807a4fe2b48de
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08211908B2

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