HCID 86756592、化合物 → HCID 22010338、化合物

HRID 322909ノート

反応式

HRID 322909 の反応式
[O:1]=[C:2]([CH2:8][C:9](=[O:33])[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]2[CH:22]=[CH:21][S:20][CH:19]=2)=[CH:12][C:11]=1[O:23][CH:24]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[CH3:32])[CH3:25])[C:3]([O:5]CC)=[O:4]>[OH-].[K+]>[O:1]=[C:2]([CH2:8][C:9](=[O:33])[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]2[CH:22]=[CH:21][S:20][CH:19]=2)=[CH:12][C:11]=1[O:23][CH:24]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[CH3:32])[CH3:25])[C:3]([OH:5])=[O:4]

参加物

3

反応物 1

HCID 86756592HCID 86756592、化合物

生成物 1

HCID 22010338HCID 22010338、化合物収率 9.8%

試薬・触媒・溶媒 1

HCID 14797Potassium Hydroxide溶媒

実験手順

A solution of ethyl (RS)-2,4-dioxo-4-[2-(1-(2-methylphenyl)ethoxy)-4-(3-thienylmethoxy)phenyl]butanoate (0.38 g) in 15% methanolic potassium hydroxide (25 mL) is stirred at reflux for 1 hour before being cooled and concentrated under reduced pressure. The residue is dissolved in water, acidified to pH 1 with concentrated hydrochloric acid and extracted with ethyl acetate. The organic layer is dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue is recrystallised from cyclohexane to give (RS)-2,4-dioxo-4-[2-(1-(2-methylphenyl)ethoxy)-4-(3-thienylmethoxy)-phenyl]butanoic acid (35 mg) as a yellow solid, m.p. 124-6° C. [Elemental analysis:- C, 65.82; H, 5.03%; Calculated for C24H22O6S:- C, 65.74; H, 5.06%].

後処理

  1. temperatureat reflux for 1 hour
  2. temperaturebefore being cooled
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue is dissolved in water
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer is dried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue is recrystallised from cyclohexane

出典と根拠

ORDレコード
ord-f6216ebce60743b097dec4fe5b0333fa
出典データセット
uspto-grants-2001_04
特許番号
US06211234B1

反応ノート

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