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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 67395719, 화합물

HRID 470606
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HRID 470606 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]=[CH:12][C:13]([OH:15])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(N1C=CN=C1)(N1C=CN=C1)=O.O[NH:29][C:30](=[NH:38])[CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.O>CN(C=O)C>[CH2:31]([C:30]1[N:38]=[C:13]([CH:12]=[CH:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[O:15][N:29]=1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 168483',4'-Dimethoxycinnamic acidHCID 682631,1'-CarbonyldiimidazoleHCID 178510798HCID 178510798, 화합물

생성물 1

HCID 67395719HCID 67395719, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-(3,4-Dimethoxy-phenyl)-acrylic acid (compound of Example 2, Method A, Step 1; 2.0 g, 9.6 mmol) was dissolved in DMF (20 mL) to which 1,1′-carbonyldiimidazole (CDI) (1.71 g, 10.56 mmol) was added and the reaction mixture was stirred at room temperature. At the end of 3 h, N-hydroxy-2-phenyl-acetamidine (1.58 g, 10.56 mmol) was added and the reaction mixture was stirred at room temperature for 8 h. After the completion of the reaction, additional CD (1.71 g, 10.56 mmol) was added and the reaction mixture was refluxed at 110° C. to 120° C. for 8 h to effect cyclodehydration. DMF was evaporated and the residue obtained was cooled to room temperature followed by addition of water (15 mL). The resulting mixture was extracted with ethyl acetate (3×10 mL). The combined organic layers were washed with water (2×10 mL) and brine (10 mL). The organic phase obtained was dried over anhydrous sodium sulfate and concentrated to afford the title compound.

후처리

  1. additionwas added
  2. stirringthe reaction mixture was stirred at room temperature for 8 h
  3. customAfter the completion of the reaction, additional CD (1.71 g, 10.56 mmol)
  4. additionwas added
  5. temperaturethe reaction mixture was refluxed at 110° C. to 120° C. for 8 h
  6. customDMF was evaporated
  7. customthe residue obtained
  8. temperaturewas cooled to room temperature
  9. extractionThe resulting mixture was extracted with ethyl acetate (3×10 mL)
  10. washThe combined organic layers were washed with water (2×10 mL) and brine (10 mL)
  11. customThe organic phase obtained
  12. dry with materialwas dried over anhydrous sodium sulfate
  13. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1eebe77d2a374c9783c401590cfc61ba
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629277B2

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