HCID 86756592, 화합물 → HCID 22010338, 화합물

HRID 322909노트

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HRID 322909 반응식
[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]

참가 물질

3

반응물 1

HCID 86756592HCID 86756592, 화합물

생성물 1

HCID 22010338HCID 22010338, 화합물수율 9.8%

시약·촉매·용매 1

HCID 14797Potassium Hydroxide용매

실험 절차

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%].

후처리

  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

출처 및 근거

ORD 기록
ord-f6216ebce60743b097dec4fe5b0333fa
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211234B1

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