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Hydrochloric Acid → HCID 4135652、化合物

HRID 850448
ノート
印刷プレビュー

反応式

HRID 850448 の反応式
[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][C:20]=1[O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[C:10]([O:12]CCCCC)=[O:11])[CH2:2][CH2:3][CH2:4][CH3:5].[OH-].[K+].Cl>CO>[CH2:1]([O:6][C:7]1[CH:8]=[C:9]([CH:18]=[CH:19][C:20]=1[O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[C:10]([OH:12])=[O:11])[CH2:2][CH2:3][CH2:4][CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19363329Pentyl 3,4-dipentyloxybenzoate

生成物 1

HCID 4135652HCID 4135652、化合物収率 70%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pentyl 3,4-dipentyloxybenzoate (911 mg, 2.50 mmol) was dissolved in methanol (15.0 ml). To this solution was added a 1N aqueous potassium hydroxide solution (7.5 ml, 7.5 mmol, 3 eq), and the mixture was stirred with reflux for 5 hours. A 3N aqueous hydrochloric acid solution was added to this reaction mixture to make the same acidic (pH <2). The mixture was extracted with chloroform (20 ml×3). The organic layer was washed with saturated brine (20 ml). The organic layer was d ried over anhydrous magnesium sulfate, and the drying agent was filtered off. The filtrate was concentrated under reduced pressure to give a colorless solid. This was recrystallized from ethyl acetate-hexane to give 3,4-dipentyloxybenzoic acid (512 mg, 70%) as colorless crystals.

後処理

  1. temperaturewith reflux for 5 hours
  2. extractionThe mixture was extracted with chloroform (20 ml×3)
  3. washThe organic layer was washed with saturated brine (20 ml)
  4. filtrationthe drying agent was filtered off
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customto give a colorless solid
  7. customThis was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-05ba9f8f246a41dfbf437ae0b213221f
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06017919

反応ノート

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