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HRID 69956作成日：2026年10月25日
1,2-Dichloroethane → Tert-butyl 6-(3-(3-amino-6-bromopicolinamido)pyridine-4-yl)-2-(trifluoromethyl)pyrimidin-4-ylcarbamate
https://huagongshe.com/reaction/69956
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | 3-Amino-6-bromopicolinic acid | HCID 45480452 | — |
| 反応物 | Tert-butyl 6-(3-aminopyridin-4-yl)-2-(trifluoromethyl)pyrimidin-4-ylcarbamate | HCID 69047673 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Tert-butyl 6-(3-(3-amino-6-bromopicolinamido)pyridine-4-yl)-2-(trifluoromethyl)pyrimidin-4-ylcarbamate | HCID 86669201 | 81% |
反応手順
A solution of tert-butyl 6-(3-aminopyridin-4-yl)-2-(trifluoro-methyl)pyrimidin-4-ylcarbamate (1.0 equiv.), 3-amino-6-bromopicolinic acid (1.0 equiv.), HOAt (1.0 equiv.), and EDC (1.0 equiv.) in DMF at a concentration of (0.2 M) was stirred for 3 hrs then heated to 50° C. overnight (homogeneous solution). Water was added to the reaction and the precipitate was filtered. The solid was further purified via SiO2 column chromatography eluting with DCM/MeOH (10%) to yield a brown solid as the desired product (81%). LCMS (m/z): 554.1/556.1 (MH+); LC Rt=3.77 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08822497B2 |
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| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-d2aa46996bb04bed9468f82fb3d01a4a |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
