Hydrochloric Acid → o-Carbamoyl-alpha-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide monohydrochloride monohydrate

HRID 1381200ノート

反応式

HRID 1381200 の反応式
C(=O)([O-])[O-:2].[K+].[K+].[C:7]([C:10]1[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=1[NH2:12])(=[O:9])[NH2:8].[CH3:17][O:18][C:19]1[CH:20]=[C:21]([CH:34]=[CH:35][C:36]=1[O:37][CH3:38])[C:22]([N:24]1[CH2:29][CH2:28][N:27]([CH2:30][C:31]([Cl:33])=[O:32])[CH2:26][CH2:25]1)=[O:23].Cl.Cl.C(O)C>O.CC(C)=O.CC(C)=O>[OH2:2].[ClH:33].[C:7]([C:10]1[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=1[NH:12][C:31](=[O:32])[CH2:30][N:27]1[CH2:28][CH2:29][N:24]([C:22](=[O:23])[C:21]2[CH:34]=[CH:35][C:36]([O:37][CH3:38])=[C:19]([O:18][CH3:17])[CH:20]=2)[CH2:25][CH2:26]1)(=[O:9])[NH2:8]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 6942AnthranilamideHCID 11430Potassium CarbonateHCID 21887872Ethanol hydrochlorideHCID 23323533[4-(3,4-Dimethoxybenzoyl)-1-piperazinyl]acetyl chloride

生成物 1

HCID 23323531o-Carbamoyl-alpha-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide monohydrochloride monohydrate

試薬・触媒・溶媒 2

HCID 180Acetone溶媒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), then 13.6 g of o-carbamoylaniline was added thereto. Under ice-cooled condition, an acetone solution of 34.4 g of [4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetyl chloride was added dropwise to the said mixture, then the reaction was carried out at a room temperature for 3 hours. Acetone was removed by distillation, the residue obtained was extracted with chloroform and the extract was washed with water, dried then chloroform was removed by distillation. The residue obtained was purified by a silica gel column chromatography, the product obtained was converted into a hydrochloride by adding hydrochloric acid-ethanol, recrystallized from water-acetone to obtain 16 g of o-carbamoyl-α-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide monohydrochloride monohydrate in the form of colorless needle-like crystals. Melting point: 122.0°-125.0° C. (decomposed).

後処理

  1. temperatureUnder ice-cooled condition
  2. customAcetone was removed by distillation
  3. customthe residue obtained
  4. extractionwas extracted with chloroform
  5. washthe extract was washed with water
  6. customdried
  7. customchloroform was removed by distillation
  8. customThe residue obtained
  9. customwas purified by a silica gel column chromatography
  10. customthe product obtained
  11. customrecrystallized from water-acetone

出典と根拠

ORDレコード
ord-6bc665541a32462597bd3a8a4da1b40b
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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