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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 67395719、化合物

HRID 470606
ノート
印刷プレビュー

反応式

HRID 470606 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 168483',4'-Dimethoxycinnamic acidHCID 682631,1'-CarbonyldiimidazoleHCID 178510798HCID 178510798、化合物

生成物 1

HCID 67395719HCID 67395719、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1eebe77d2a374c9783c401590cfc61ba
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629277B2

反応ノート

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