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Hydrochloric Acid → HCID 53635745、化合物

HRID 395675
ノート
印刷プレビュー

反応式

HRID 395675 の反応式
[CH3:1][O:2][C:3]1[CH:33]=[CH:32][C:6]([C:7]([NH:9][C:10]2[C:11]([NH:16][C:17]([CH:19]3[CH2:24][CH2:23][N:22](CC4C=CC=CC=4)[CH2:21][CH2:20]3)=[O:18])=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:5][CH:4]=1.Cl>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([NH:9][C:10]2[C:11]([NH:16][C:17]([CH:19]3[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]3)=[O:18])=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:32][CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 9824675HCID 9824675、化合物

生成物 1

HCID 53635745HCID 53635745、化合物収率 81%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of N1-(4-methoxybenzoyl)-N2-(1-benzylpiperidin-4-ylcarbonyl)-1,2-benzenediamine (1.02 g, 2.30 †mmol), 1 N aqueous hydrochloric acid (5 mL), and 5% pallidium-on-carbon (1.06 g) in ethanol (100 mL) was placed under a hydrogen atmosphere (1 bar). After 16 h, the mixture was filtered through diatomaceous earth and the filtrate concentrated in vacuo. The residue was treated with 1 N aqueous sodium hydroxide followed by ethyl acetate. The aqueous layer was extracted twice with ethyl acetate and the combined organics were washed with 1 N aqueous sodium hydroxide, saturated sodium chloride solution, and dried (potassium carbonate). Concentration and recrystallization yielded 656 mg (81%) of the title compound.

後処理

  1. filtrationthe mixture was filtered through diatomaceous earth
  2. concentrationthe filtrate concentrated in vacuo
  3. additionThe residue was treated with 1 N aqueous sodium hydroxide
  4. extractionThe aqueous layer was extracted twice with ethyl acetate
  5. washthe combined organics were washed with 1 N aqueous sodium hydroxide, saturated sodium chloride solution
  6. dry with materialdried (potassium carbonate)
  7. concentrationConcentration and recrystallization

出典と根拠

ORDレコード
ord-d1551d62dae542f3aeed65c909e342e9
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06605626B2

反応ノート

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