5-n-butyl-2,4-dihydro-2-[1-(N-methylcarbamoyl)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one → HCID 178441927, 화합물

HRID 36218

반응식

HRID 36218 반응식
[CH2:1]([C:5]1[N:6]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]#[N:31])=[CH:20][CH:19]=2)[C:7](=[O:16])[N:8]([CH:10]([C:12](=[O:15])[NH:13][CH3:14])[CH3:11])[N:9]=1)[CH2:2][CH2:3][CH3:4].[NH:32]1C=N[N:34]=[N:33]1>C(Cl)Cl>[CH2:1]([C:5]1[N:6]([CH2:17][C:18]2[CH:19]=[CH:20][C:21]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]3[NH:34][N:33]=[N:32][N:31]=3)=[CH:22][CH:23]=2)[C:7](=[O:16])[N:8]([CH:10]([C:12](=[O:15])[NH:13][CH3:14])[CH3:11])[N:9]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 199394395-n-butyl-2,4-dihydro-2-[1-(N-methylcarbamoyl)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-oneHCID 178418441HCID 178418441, 화합물

생성물 1

HCID 178441927HCID 178441927, 화합물수율 43%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
120 °C

실험 절차

The conversion of 5-n-butyl-2,4-dihydro-2-[1-(N-methylcarbamoyl)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one to the corresponding tetrazole was accomplished by the procedure of Example 9, Step E, except that the mixture was stirred at 120° C. for 2 days. After work-up, the residue was taken up in CH2Cl2 and flash chromatographed over silica gel (15 mL for 0.19 mmole, gradient elution using 5-30% MeOH/CH2Cl2 to give the desired compound as a white powder in 43% yield, homogeneous by TLC in 30% MeOH/CH2Cl2, mass spectrum (FAB) 461 (M+1)+, mp 153°-155° C.

후처리

  1. customflash chromatographed over silica gel (15 mL
  2. washfor 0.19 mmole, gradient elution

출처 및 근거

ORD 기록
ord-235f2d3ec61644bd9e14d82e7ad6db05
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05411980

연결된 노트

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