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Potassium Hydroxide → HCID 21180559、化合物

HRID 1386446
ノート
印刷プレビュー

反応式

HRID 1386446 の反応式
[OH-].[K+].C([O:5][C:6](=[O:32])[C:7]1[C:12]([O:13][C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)=[CH:11][CH:10]=[CH:9][C:8]=1[O:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=1)C>CO>[CH2:21]1[O:20][C:17]2[CH:18]=[CH:19][C:14]([O:13][C:12]3[CH:11]=[CH:10][CH:9]=[C:8]([O:23][C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=4)[C:7]=3[C:6]([OH:32])=[O:5])=[CH:15][C:16]=2[O:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 21180554HCID 21180554、化合物

生成物 1

HCID 21180559HCID 21180559、化合物収率 67.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

KOH (371 mg, 5.7 mmol) that was dissolved in methanol was added to a solution of ethyl-2-(3-methoxyphenoxy)-6-[3,4-(methylenedioxy)phenoxy]benzoate (200 mg, 0.57 mmol) in methanol (5 ml). The mixture was heated under reflux for approximately 20 hours at which time TLL had indicated the formation of a polar material. The solvent was evaporated and the remaining residue was diluted with water (7 ml, pH≈7.5) and extracted with EtOAc (2×10 ml). The aqueous fraction was then acidified to pH˜2.5 using concentrated HCl and then extracted with ethyl acetate (2×10 ml). Evaporation of solvents gave an off-white solid which was recrystallized from methanol/H2O to give 146 mg (67%) of a white solid, mp 146-148° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for approximately 20 hours at which time TLL
  3. customThe solvent was evaporated
  4. additionthe remaining residue was diluted with water (7 ml, pH≈7.5)
  5. extractionextracted with EtOAc (2×10 ml)
  6. extractionextracted with ethyl acetate (2×10 ml)
  7. customEvaporation of solvents
  8. customgave an off-white solid which
  9. customwas recrystallized from methanol/H2O

出典と根拠

ORDレコード
ord-c606fcb109be4a889c1c4b242ed12141
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06265428B1

反応ノート

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