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Ethyl 2-oxocyclopentanecarboxylate → HCID 136203297、化合物

HRID 1508920
ノート
印刷プレビュー

反応式

HRID 1508920 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 136203297HCID 136203297、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-990ed41c409748f09eca8cb1d44d34d6
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221843B2

反応ノート

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