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Water → HCID 14552389, 화합물

HRID 1110778
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HRID 1110778 반응식
[CH2:1]([NH:4][C@@H:5]1[CH2:14][CH2:13][C:8]2([O:12][CH2:11][CH2:10][O:9]2)[CH2:7][C@H:6]1[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:2][CH3:3].[C:20]([O:24][CH2:25][CH3:26])(=[O:23])[CH:21]=[CH2:22].O>C(O)C>[CH2:25]([O:24][C:20](=[O:23])[CH2:21][CH2:22][N:4]([CH2:1][CH2:2][CH3:3])[C@@H:5]1[CH2:14][CH2:13][C:8]2([O:12][CH2:11][CH2:10][O:9]2)[CH2:7][C@H:6]1[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 8821Ethyl Acrylate3회HCID 14552387HCID 14552387, 화합물

생성물 1

HCID 14552389HCID 14552389, 화합물수율 59.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 8-(propylamino)-trans-1,4-dioxaspiro[4.5]-decane-7-carboxylate (129.6 g, 0.48 mole) was dissolved in ethanol (1500 ml), then ethyl acrylate (479 g, 4.8 mole) was added. The mixture was refluxed overnight, then additional ethyl acrylate (479 g, 4.8 mole) was added. The mixture was refluxed for 24 hours, at which time a third addition of ethyl acrylate (479 g, 0.48 mole) was made, followed by 60 hours of reflux. The mixture was then cooled to room temperature, poured into water, and the hydrogen ion concentration was adjusted to pH 10. The product was extracted with methylene chloride, dried with sodium sulfate and evaporated to give 177.4 g of crude product. This was purified by HPLC to give 102.1 g of the title product (59.8%).

후처리

  1. temperatureThe mixture was refluxed overnight
  2. temperatureThe mixture was refluxed for 24 hours, at which time
  3. temperatureof reflux
  4. concentrationthe hydrogen ion concentration
  5. extractionThe product was extracted with methylene chloride
  6. dry with materialdried with sodium sulfate
  7. customevaporated
  8. customto give 177.4 g of crude product
  9. customThis was purified by HPLC

출처 및 근거

ORD 기록
ord-49611422efaf4150a833c52acc4ab701
출처 데이터셋
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04977160

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