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4-Hydroxybenzoic Acid → HCID 53969391、化合物

HRID 864611
ノート
印刷プレビュー

反応式

HRID 864611 の反応式
S(C1C=CC(C)=CC=1)(O[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]=[CH2:15])(=O)=O.OC1C=CC(C(O)=O)=CC=1.[Cl:33][C:34]1[CH:35]=[C:36]([CH:40]=[CH:41][C:42]=1[OH:43])[C:37]([OH:39])=[O:38].[OH-].[K+]>C(O)C>[Cl:33][C:34]1[CH:35]=[C:36]([CH:40]=[CH:41][C:42]=1[O:43][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH:6]=[CH2:5])[C:37]([OH:39])=[O:38]
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 1354-Hydroxybenzoic Acid2 回HCID 14797Potassium Hydroxide2 回HCID 198603-Chloro-4-hydroxybenzoic acidHCID 11141895HCID 11141895、化合物

生成物 1

HCID 53969391HCID 53969391、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

10-Undecen-1-yl Tosylate (compound I-7) was separately reacted with 4-hydroxybenzoic acid and 3-chloro-4-hydroxy-benzoic acid to synthesize the compounds I-18 and I-19. The synthesis of compound I-18 was described below as an example. 1.75 g (0.0312 mole) KOH, 0.05 g KI and 100 ml of 90% ethanol were mixed and refluxed. To the mixture 2.15 g (0.0156 mole) 4-hydroxybenzoic acid was added dropwise, and refluxed for one hour. 4.433 g (0.013 mole) compound I-7 was added slowly and refluxed for 10 hours. 10% KOH was then added and refluxed again for two hours. Ethanol was removed from the mixture which was then extracted with ethyl ether. The collected ethyl ether layer was dried over anhydrous MgSO4, filtered and concentrated to obtained solid product. The resulting solid product was recrystallized from ethanol. Yield: I-18: 40.6%; I-19: 36.4%. 1H-NMR:

後処理

  1. customto synthesize the compounds
  2. customThe synthesis of compound I-18
  3. temperaturerefluxed
  4. temperaturerefluxed for one hour
  5. temperaturerefluxed for 10 hours
  6. temperaturerefluxed again for two hours
  7. customEthanol was removed from the mixture which
  8. extractionwas then extracted with ethyl ether
  9. dry with materialThe collected ethyl ether layer was dried over anhydrous MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customto obtained solid product
  13. customThe resulting solid product was recrystallized from ethanol

出典と根拠

ORDレコード
ord-90230dfae7a241ddbe8fffe2b399769e
出典データセット
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05563230

反応ノート

読み込み中…

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