Hydrochloric Acid → Diethyl 2-acetyl-2-phenylmalonate

HRID 270222

반응식

HRID 270222 반응식
[C:1]1([CH:7]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O-:18][CH2:19][CH3:20].[Na+].C(Cl)(=O)C.Cl>O1CCCC1>[C:19]([C:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)([C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:13]([O:15][CH2:16][CH3:17])=[O:14])(=[O:18])[CH3:20]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 66514Diethyl phenylmalonateHCID 2723922Sodium ethoxide

생성물 1

HCID 21964398Diethyl 2-acetyl-2-phenylmalonate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of diethyl 2-phenylmalonate (100 mmol) in anhydrous tetrahydrofuran (300 mL) is added sodium ethoxide (110 mmol). The mixture is stirred at room temperature for 30 min, followed by the addition of a solution of acetyl chloride (110 mmol) in tetrahydrofuran (50 mL). After the addition is complete, the mixture is heated to reflux for 3 hours, cooled to room temperature, neutralized with 2 N HCl, then concentrated in vacuo. The residue is partitioned between H20 and CHCl3, the organic extracts washed with sodium bicarbonate, water, and brine, dried (MgS04), filtered and concentrated.

후처리

  1. additionAfter the addition
  2. temperaturethe mixture is heated
  3. temperatureto reflux for 3 hours
  4. temperaturecooled to room temperature
  5. concentrationconcentrated in vacuo
  6. customThe residue is partitioned between H20 and CHCl3
  7. washthe organic extracts washed with sodium bicarbonate, water, and brine
  8. customdried (MgS04)
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d547d0bd329247e984fcbcf80508e4fb
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449490B2

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