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

HRID 261053노트

반응식

HRID 261053 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-8f5b826705344d14976ac03bc8e97a47
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04163789

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