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1,2-Dichloroethane → Tert-butyl 3-(4-(3-nitropyridin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | N-((1,1-dimethylethoxy)carbonyl)-beta-alanine | HCID 76809 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | 1-(3-Nitropyridin-4-yl)piperazine | HCID 43114071 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Tert-butyl 3-(4-(3-nitropyridin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate | HCID 69044068 | 93% |
反応手順
A solution containing 1.0 eq each of 1-(3-nitropyridin-4-yl)piperazine, N-Boc-beta-alanine, HOAT and EDC in DCM, at a concentration of 0.1 M, was stirred for 16 hours. The solution was diluted with EtOAc and was washed with H2O, Na2CO3(sat), NaCl(sat.), was dried over MgSO4, was filtered and the volatiles were removed in vacuo yielding tert-butyl 3-(4-(3-nitropyridin-4-yl)piperazin-1-yl)-3-oxopropylcarbamate (93%). LCMS (m/z): 379.9 (MH+); LC Rt=1.92 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822497B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-15eb03f88afe4dd7b5b57a57fa19cdb4 |
| 出典メモ | uspto-grants-2014_09 |