Diethyl Ether → N-[1-(alpha-(2-(2-(2-Methoxyethoxy)-ethoxy)-ethoxycarbonyloxy)benzyl)-1,4-dihydropyridin-4-ylidene]-N'-cyano-N''-(6-(4-chlorophenoxy)-hexyl)-guanidine

HRID 1060789

반응식

HRID 1060789 반응식
[Cl:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14]([NH:22][C:23]#[N:24])=[N:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)=[CH:4][CH:3]=1.[C:27](=[O:48])([O:37][CH2:38][CH2:39][O:40][CH2:41][CH2:42][O:43][CH2:44][CH2:45][O:46][CH3:47])[O:28][CH:29](Cl)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.CCOC(C)=O.CCOCC>ClCCl>[CH3:47][O:46][CH2:45][CH2:44][O:43][CH2:42][CH2:41][O:40][CH2:39][CH2:38][O:37][C:27]([O:28][CH:29]([N:19]1[CH:20]=[CH:21][C:16](=[N:15][C:14]([NH:22][C:23]#[N:24])=[N:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][O:6][C:5]2[CH:25]=[CH:26][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH:17]=[CH:18]1)[C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1)=[O:48]

참가 물질

6

반응물 4

HCID 3283Diethyl Ether2회HCID 8857Ethyl AcetateHCID 18629469alpha-Chlorobenzyl 2-(2-(2-methoxyethoxy)-ethoxy)-ethyl carbonateHCID 178512290Chs-828

생성물 1

HCID 10168663N-[1-(alpha-(2-(2-(2-Methoxyethoxy)-ethoxy)-ethoxycarbonyloxy)benzyl)-1,4-dihydropyridin-4-ylidene]-N'-cyano-N''-(6-(4-chlorophenoxy)-hexyl)-guanidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of N-(6-(4-chlorophenoxy)-hexyl)-N′-cyano-N″-(4-pyridyl)-guanidine (67 mg) and α-chlorobenzyl 2-(2-(2-methoxyethoxy)-ethoxy)-ethyl carbonate (150 mg) was placed in a preheated oil bath at 90° C. After 10 minutes a clear yellow melt was formed and after a further 20 minutes the mixture was cooled to room temperature and EtOAc (4 ml) was added. Decantation and evaporation in vacuo gave a residue which was treated with ether. After decantation of the ether, the residue was taken up in dichloromethane and washed with an excess of sodium bicarbonate. Chromatography on silica gel with dichloromethane/methanol (98:2) as eluent gave the title compound as a colourless oil.

후처리

  1. customwas placed in a preheated oil bath at 90° C
  2. customAfter 10 minutes a clear yellow melt was formed and after a further 20 minutes the mixture
  3. customDecantation and evaporation in vacuo
  4. customgave a residue which
  5. washwashed with an excess of sodium bicarbonate

출처 및 근거

ORD 기록
ord-5e422d87fc5f4d0882780eb4bd096495
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525077B2

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