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Triethylamine → Methyl 2-({[2-(dimethylamino)-2-oxoethyl]carbamoyl}amino)-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 2-Amino-N,N-dimethylacetamide acetate | HCID 53399009 | — |
| 反応物 | Methyl 2-amino-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate | HCID 66653263 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Methyl 2-({[2-(dimethylamino)-2-oxoethyl]carbamoyl}amino)-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate | HCID 66652958 | 143.4% |
反応手順
0.798 g (2.69 mmol) of triphosgene diluted in 10 ml of dioxane is added, under an inert atmosphere at ambient temperature, to 1.3 g (3.84 mmol) of methyl 2-amino-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate in 50 ml of dioxane. After stirring for 1 hour, 1.25 g (7.68 mmol) of N,N-dimethylglycinamide acetate and 2.68 ml (19.21 mmol) of triethylamine are added. The reaction medium is stirred overnight at ambient temperature and then hydrolysed with water. The aqueous phase is extracted with dichloromethane. The organic phase obtained is dried over sodium sulphate, filtered, and then concentrated under reduced pressure. 1.8 g of a yellow solid are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859544B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-7fe39e2e149f470199cb02595e447c39 |
| 出典メモ | uspto-grants-2014_10 |