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Ethyl 2-oxocyclopentanecarboxylate → HCID 136203297, 화합물

HRID 1508920
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HRID 1508920 반응식
Cl.[CH:2]1([C:7](=[NH:9])[NH2:8])[CH2:6][CH2:5][CH2:4][CH2:3]1.O=[C:11]1[CH2:15][CH2:14][CH2:13][CH:12]1[C:16](OCC)=[O:17].C[O-].[Na+]>C(O)C>[CH:2]1([C:7]2[NH:9][C:16](=[O:17])[C:12]3[CH2:13][CH2:14][CH2:15][C:11]=3[N:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3]1
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참가 물질

5

반응물 3

HCID 69136Ethyl 2-oxocyclopentanecarboxylateHCID 10942334Sodium MethoxideHCID 42614157Cyclopentanecarboximidamide hydrochloride

생성물 1

HCID 136203297HCID 136203297, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A 250-mL round bottomed flask was charged with cyclopentanecarboximidamide hydrochloride (5.38 g, 36.2 mmol), ethyl 2-oxocyclopentanecarboxylate (5.14 g, 38.7 mmol), and ethanol (100 mL). To the stirred mixture at rt was added sodium methoxide (3.91 g, 72.4 mmol). The resulting mixture was stirred under reflux for 22 h. After cooling to room temperature, the mixture was evaporated under reduced pressure to 25 mL. The residual slurry was cautiously treated with 2N HCl (50 mL). The solution was extracted with ethyl acetate (4×50 mL). The combined extract was washed with saturated sodium chloride (2×25 mL), dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford the title compound which was carried forward into the next step without further purification.

후처리

  1. temperatureunder reflux for 22 h
  2. customthe mixture was evaporated under reduced pressure to 25 mL
  3. additionThe residual slurry was cautiously treated with 2N HCl (50 mL)
  4. extractionThe solution was extracted with ethyl acetate (4×50 mL)
  5. extractionThe combined extract
  6. washwas washed with saturated sodium chloride (2×25 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-990ed41c409748f09eca8cb1d44d34d6
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221843B2

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