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Morpholine → Ethyl alpha-oxo-4-morpholineacetate

HRID 1777221
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HRID 1777221 반응식
Cl[C:2](=[O:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.C(N(CC)CC)C>C(OCC)C>[O:12]1[CH2:13][CH2:14][N:9]([C:2](=[O:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH2:10][CH2:11]1
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참가 물질

5

반응물 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 20884Ethoxalyl chloride

생성물 1

HCID 3414011Ethyl alpha-oxo-4-morpholineacetate수율 58.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of ethyl 2-chloro-2-oxoacetate (1.25 g, 9.18 mmol) in diethyl ether (5 mL) was added dropwise to a solution of morpholine (1.0 g, 11.48 mmol) in diethyl ether (20 mL) and triethylamine (1.16 g, 11.48 mmol) at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 2 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The yellow-colored oil was transferred into 25 mL iced water and extracted with ethyl acetate (3×20 mL). Combined organic layers were washed with brine, dried over anhydrous sodium sulphate, and concentrated under reduced pressure to give 1 g of the crude product, which was used further without any purification. Crude yield 47%. 1H NMR (400 MHz, CDCl3) δ 4.33-4.38 (q, 2H), 3.72-3.76 (m, 4H), 3.65-3.68 (m, 2H), 3.47-3.50 (m, 2H), 1.37-1.40 (t, 3H). LCMS m/z 187.93 [M+H]+, tR=0.525 min.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. extractionextracted with ethyl acetate (3×20 mL)
  4. washCombined organic layers were washed with brine
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-53db62a00a914d73bb8fce213e49c5ab
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266843B2

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