Diethyl benzamidomalonate → HCID 21866624, 화합물

HRID 857208

반응식

HRID 857208 반응식
[O-][CH2:2]C.[Na+].C(O)C.[C:8]([NH:16][CH:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:18]([O:20][CH2:21][CH3:22])=[O:19])(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Br[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][O:35][C:36]([CH3:42])([CH3:41])[C:37]([O:39][CH3:40])=[O:38]>C(O)C>[C:8]([NH:16][C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][O:35][C:36]([CH3:42])([CH3:41])[C:37]([O:39][CH2:40][CH3:2])=[O:38])(=[O:15])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 66790Diethyl benzamidomalonateHCID 21866674Methyl 6-bromohexyloxy-2-methylpropionateHCID 23706232Ethanol sodium ethoxide

생성물 1

HCID 21866624HCID 21866624, 화합물수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To 5 ml of dry ethanol, 675 mg of 20% sodium ethoxide-ethanol solution and 698 mg of diethyl benzoylaminomalonate were added, and stirred for 30 minutes at room temperature. Then, a solution of 914 mg of methyl 6-bromohexyloxy-2-methylpropionate/4 ml of dry ethanol was added dropwise, and stirred for 15 hours at 50-60° C. The reaction solution was poured into ice-cold water and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (Wakogel® C-200, n-hexane: ethyl acetate=5:1) to provide 642 mg of the objective compound as yellowish oil.

후처리

  1. stirringstirred for 15 hours at 50-60° C
  2. additionThe reaction solution was poured into ice-cold water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography (Wakogel® C-200, n-hexane: ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-3beecc5c37d045718007a558cfddd25b
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07144906B2

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