Asulam → Methyl 4-(3-(3,4-dichlorobenzyl)ureido)phenylsulfonylcarbamate

HRID 215904

반응식

HRID 215904 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12](=[O:15])[O:13][CH3:14])(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(N(CC)C(C)C)(C)C.[Cl:25][C:26]1[CH:27]=[C:28]([CH:33]=[CH:34][C:35]=1[Cl:36])[CH2:29][N:30]=[C:31]=[O:32]>C(#N)C>[Cl:25][C:26]1[CH:27]=[C:28]([CH:33]=[CH:34][C:35]=1[Cl:36])[CH2:29][NH:30][C:31](=[O:32])[NH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12](=[O:15])[O:13][CH3:14])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 18752AsulamHCID 81531DiisopropylethylamineHCID 27333681,2-Dichloro-4-(isocyanatomethyl)benzene

생성물 1

HCID 25120648Methyl 4-(3-(3,4-dichlorobenzyl)ureido)phenylsulfonylcarbamate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of methyl 4-aminophenylsulfonylcarbamate (50 mg, 0.2 mmol), N,N-diisopropylethylamine (35 L, 0.2 mmol), 3,4-dichlorobenzylisocyanate (30 L, 0.2 mmol) in acetonitrile was stirred under an N2 atmosphere for 19 h. The mixture was concentrated and the residue purified by reverse phase HPLC using 10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA) to give methyl 4-(3-(3,4-dichlorobenzyl)ureido)phenylsulfonylcarbamate. LC/MS (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)), m/z: M+1 obs=431.01; tR=2.9 min.

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue purified by reverse phase

출처 및 근거

ORD 기록
ord-f08f4c057fcb4e8cbe50d5cae9e78d17
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193194B2

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