Hydrochloric Acid → Diethyl 2-acetyl-2-phenylmalonate

HRID 270222

反応式

HRID 270222 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 21964398Diethyl 2-acetyl-2-phenylmalonate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d547d0bd329247e984fcbcf80508e4fb
出典データセット
uspto-grants-2008_11
特許番号
US07449490B2

関連ノート

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