Water → 4-(Diethylcarbamoyl)benzoic acid

HRID 1934768노트

반응식

HRID 1934768 반응식
[CH2:1]([N:3]([CH2:16][CH3:17])[C:4]([C:6]1[CH:15]=[CH:14][C:9]([C:10]([O:12]C)=[O:11])=[CH:8][CH:7]=1)=[O:5])[CH3:2].[OH-].[Na+].O.C(OCC)(=O)C>CO>[CH2:16]([N:3]([CH2:1][CH3:2])[C:4]([C:6]1[CH:15]=[CH:14][C:9]([C:10]([OH:12])=[O:11])=[CH:8][CH:7]=1)=[O:5])[CH3:17]

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 14434573Methyl 4-(diethylcarbamoyl)benzoate

생성물 1

HCID 125534994-(Diethylcarbamoyl)benzoic acid수율 57.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 25 ml of methanol was dissolved 5.44 g of methyl 4-[(diethylamino)carbonyl]-benzoate. After adding 25 ml of 1 mol/L aqueous solution of sodium hydroxide at 0-5° C., the mixture was stirred at ambient temperature for 2 hours. The reaction mixture was poured into a mixture of water and ethyl acetate, and the aqueous layer was separated. The aqueous layer was mixed with ethyl acetate, pH was adjusted to 1.5 with 6 mol/L hydrochloric acid, and the organic layer was separated. The organic layer was washed successively with water and saturated aqueous solution of sodium chloride and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. Diisopropyl ether was added to the residue, and the deposited crystal was collected by filtration to obtain 2.94 g of 4-[(diethylamino)carbonyl]-benzoic acid as a colorless crystalline product.

후처리

  1. customthe aqueous layer was separated
  2. additionThe aqueous layer was mixed with ethyl acetate, pH
  3. customthe organic layer was separated
  4. washThe organic layer was washed successively with water and saturated aqueous solution of sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionDiisopropyl ether was added to the residue
  8. filtrationthe deposited crystal was collected by filtration

출처 및 근거

ORD 기록
ord-a73c6c33333040188faa9960f2a7505a
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06384065B1

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