Ethanol → N-(1-Cyclohexylmethylpiperid-4-yl)-2-methoxy-4-amino-5-chlorobenzamide

HRID 261053ノート

反応式

HRID 261053 の反応式
[CH:1]1([CH2:7][N:8]2[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:32])[C:16]3[CH:21]=[C:20]([Cl:22])[C:19]([NH:23]C(=O)C(F)(F)F)=[CH:18][C:17]=3[O:30][CH3:31])[CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(O)C.[OH-].[Na+]>O>[CH:1]1([CH2:7][N:8]2[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:32])[C:16]3[CH:21]=[C:20]([Cl:22])[C:19]([NH2:23])=[CH:18][C:17]=3[O:30][CH3:31])[CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 20395852N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-trifluoroacetamido-5-chlorobenzamide

生成物 1

HCID 20395834N-(1-Cyclohexylmethylpiperid-4-yl)-2-methoxy-4-amino-5-chlorobenzamide収率 77.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-trifluoroacetamido-5-chlorobenzamide (8.1 g; 0.017 moles), ethanol (25 ml), water (15 ml) and 8 N sodium hydroxide aqueous solution (25 ml) was stirred for 12 hours at room temperature. After dilution with water, the mixture was extracted with chloroform and the chloroformic solution dried (Na2SO4) and evaporated in vacuo. N-(1-Cyclohexylmethylpiperid-4-yl)-2-methoxy-4-amino-5-chlorobenzamide (5 g) was obtained. It was converted into its hydrochloride by treatment with a saturated solution of ethanolic hydrogen chloride; the hydrochloride melted at 225°-227° C. (dec).

後処理

  1. extractionAfter dilution with water, the mixture was extracted with chloroform
  2. dry with materialthe chloroformic solution dried (Na2SO4)
  3. customevaporated in vacuo

出典と根拠

ORDレコード
ord-8f5b826705344d14976ac03bc8e97a47
出典データセット
uspto-grants-1979_08
特許番号
US04163789

反応ノート

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