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Potassium Iodide → cis-4-amino-5-chloro-N-[1-[2-(1,4-dihydro-2,4-dioxo-3(2H)-quinazolinyl)ethyl]-3-methoxy-4-piperidinyl]-2-methoxybenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 3-(2-chloroethyl)(1H,3H)quinazoline-2,4-dione | HCID 78766 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Amino-5-chloro-2-methoxy-N-[(3R,4S)-3-methoxypiperidin-4-YL]benzamide | HCID 9861621 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | cis-4-amino-5-chloro-N-[1-[2-(1,4-dihydro-2,4-dioxo-3(2H)-quinazolinyl)ethyl]-3-methoxy-4-piperidinyl]-2-methoxybenzamide | HCID 15096932 | — |
反応手順
A mixture of 3.8 parts of 3-(2-chloroethyl)-2(1H), 4(3H)-quinazolinedione, 4.7 parts of cis-4-amino-5-chloro-2-methoxy-N-(3-methoxy-4-piperidinyl)benzamide, 1.7 parts of sodium hydrogen carbonate, 0.1 parts of potassium iodide and 160 parts of 4-methyl-2-pentanone was stirred and refluxed for 24 hours. Water was added to the reaction mixture. The precipitated product was filtered off and crystallized from N,N-dimethylformamide and a small amount of water, yielding 3.3 parts of cis-4-amino-5-chloro-N-[1-[2-(1,4-dihydro-2,4-dioxo-3(2H)-quinazolinyl)ethyl]-3-methoxy-4-piperidiny]-2-methoxybenzamide; mp. 270.8° C. (compound 142).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04962115 |
| 出典データセット | uspto-grants-1990_10 |
| ORD ID | ord-022d02862e7943faa08f947abacb089a |
| 出典メモ | uspto-grants-1990_10 |