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

HRID 261052
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HRID 261052 반응식
O.Cl.[CH:3]1([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([NH:16][C:17](=[O:31])[C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([NH:25]C(=O)C)=[CH:20][C:19]=3[O:29][CH3:30])[CH2:12][CH2:11]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.Cl.[OH-].[Na+]>O>[CH:3]1([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([NH:16][C:17](=[O:31])[C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([NH2:25])=[CH:20][C:19]=3[O:29][CH3:30])[CH2:12][CH2:11]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 20395819N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide hydrochloride monohydrate

생성물 1

HCID 20395834N-(1-Cyclohexylmethylpiperid-4-yl)-2-methoxy-4-amino-5-chlorobenzamide수율 93.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide hydrochloride monohydrate (10 g; 0.02 moles), concentrated hydrochloric acid (6 ml) and water (20 ml) was boiled under reflux for 1.5 hours. The solution was then made alkaline with sodium hydroxide solution and extracted with chloroform. The organic solution was dried (Na2SO4) and the solvent removed in vacuo to give N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-amino-5-chlorobenzamide (7.1 g), m.p. 213°-215° C. after recrystallization from methanol.

후처리

  1. temperatureunder reflux for 1.5 hours
  2. extractionextracted with chloroform
  3. dry with materialThe organic solution was dried (Na2SO4)
  4. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-ea3189585c4543bfb2f4d3f7e4cc3f9e
출처 데이터셋
uspto-grants-1979_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04163789

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