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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acrylonitrile → HCID 67358715, 화합물

HRID 2408823
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인쇄 미리보기

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HRID 2408823 반응식
[C:1]1([CH:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O-]CC.[Na+].[C:23](#[N:26])[CH:24]=[CH2:25]>O1CCOCC1>[C:23]([CH2:24][CH2:25][C:7]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:8]([O:10][CH2:11][CH3:12])=[O:9])#[N:26]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7855AcrylonitrileHCID 226748Ethyl diphenylacetateHCID 2723922Sodium ethoxide

생성물 1

HCID 67358715HCID 67358715, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
45 °C

실험 절차

The product of Example 1A (5.58 g) was dissolved in anhydrous dioxane (15 mL). Sodium ethoxide (1.58 g) was added, and the mixture was heated to 40-50° C. for 30 minutes. Acrylonitrile (1.44 mL) was added dropwise with stirring. The mixture was heated at 60-70° C. for one hour. The dioxane was removed in vacuo, and the residue was taken up in diethyl ether, washed with water and brine, dried with magnesium sulfate, filtered, and concentrated. The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane) to obtain the title compound. MS (DCI+) m/z 311 (M+NH4)+.

후처리

  1. temperatureThe mixture was heated at 60-70° C. for one hour
  2. customThe dioxane was removed in vacuo
  3. washwashed with water and brine
  4. dry with materialdried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-8657960009884f52895690af334d4bf9
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815869B2

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