Acetone → Acetanilide

HRID 1381195ノート

反応式

HRID 1381195 の反応式
C(=O)([O-])[O-].[K+].[K+].COC([C:11]1[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=1[NH2:13])=O.[CH3:18][C:19](C)=[O:20].COC1C=C(C=CC=1OC)C(N1CCN(CC(Cl)=O)CC1)=O>O.CC(C)=O>[C:19]([NH:13][C:12]1[CH:11]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:20])[CH3:18]

参加物

6

反応物 4

HCID 180AcetoneHCID 8635Methyl AnthranilateHCID 11430Potassium CarbonateHCID 23323533[4-(3,4-Dimethoxybenzoyl)-1-piperazinyl]acetyl chloride

生成物 1

HCID 904Acetanilide

試薬・触媒・溶媒 1

HCID 18366337Propan-2-one--water (1/1)溶媒

実験手順

8.28 Grams of potassium carbonate was dissolved in 50 ml of water-acetone (1:2), and to this solution was added 15.1 g of o-methoxycarbonylaniline. Under ice-cooled condition, an acetone solution of 34.4 g of [4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetylchloride was added dropwise thereto. After completion of the addition, the reaction was carried out at a room temperature for 3 hours, then acetone was removed by distillation. The residue obtained was extracted with chloroform, then the extract was washed with water, dried and chloroform was removed by distillation. The residue obtained was crystallized by adding ethyl acetate, and the crystals were collected by filtration. Recrystallized from ethanol to obtain 29 g o-methoxycarbonyl-α-[4-3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide in the form of colorless needle-like crystals. Melting point: 167.5°-169.0° C.

後処理

  1. temperatureUnder ice-cooled condition
  2. additionAfter completion of the addition
  3. customacetone was removed by distillation
  4. customThe residue obtained
  5. extractionwas extracted with chloroform
  6. washthe extract was washed with water
  7. customdried
  8. customchloroform was removed by distillation
  9. customThe residue obtained
  10. customwas crystallized
  11. additionby adding ethyl acetate
  12. filtrationthe crystals were collected by filtration
  13. customRecrystallized from ethanol

出典と根拠

ORDレコード
ord-f0797784d47b4f8a9500af4d742d99bb
出典データセット
uspto-grants-1986_04
特許番号
US04585774

反応ノート

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