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Asulam → Methyl 4-(3-(3,4-dichlorobenzyl)ureido)phenylsulfonylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Asulam | HCID 18752 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,2-Dichloro-4-(isocyanatomethyl)benzene | HCID 2733368 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 4-(3-(3,4-dichlorobenzyl)ureido)phenylsulfonylcarbamate | HCID 25120648 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08883766B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-4717ed95419a4007a1a499480128a54d |
| 出典メモ | uspto-grants-2014_11 |