Hydrochloric Acid → HCID 54285185, 화합물

HRID 249554노트

반응식

HRID 249554 반응식
C[C:2]1(C)[O:6][CH:5]([CH2:7][C:8](=[O:15])[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:4](=[O:16])[O:3]1.Cl>C1(C)C=CC=CC=1.C[O-].[Na+]>[OH:6][CH:5]([CH2:7][C:8](=[O:15])[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:4]([O:3][CH3:2])=[O:16]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 19761817HCID 19761817, 화합물

생성물 1

HCID 54285185HCID 54285185, 화합물수율 84.8%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 10942334Sodium Methoxide용매

실험 절차

To a solution of ethyl 4-(2,2-dimethyl-5-oxo-1,3-dioxolan-4-yl)-3-oxobutanoate (480 mg, 1.97 mmol) in toluene (2.0 ml), sodium methoxide (1M in methanol) (2.1 ml) was dropwise added at 0° C. in an argon atmosphere and stirred for 30 minutes. To the mixture, 1N hydrochloric acid (2.1 ml) was dropwise added and the mixture was stirred at room temperature for 15 minutes. After evaporating off the most of the organic solvent under reduced pressure, the mixture was extracted with ethyl acetate and washed with a saturated saline and a phosphate buffer (pH 7.0). The organic layers were combined, dried over sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (hexane:ethyl acetate=5:1) to give pure 1-methyl 6-ethyl 2-hydroxy-4-oxoadipate (366 mg, 1.67 mmol). Yield, 85 %.

후처리

  1. stirringthe mixture was stirred at room temperature for 15 minutes
  2. customAfter evaporating off the most of the organic solvent under reduced pressure
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with a saturated saline
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a3b7dbd6fd97436889d83a527cc76e0e
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05214197

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