関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Esomeprazole BINOL | HCID 178488158 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | HCID 178488037 | HCID 178488037 | — |
反応手順
Esomeprazole-BINOL inclusion complex (100 g; 158.3 mmol; ee of 98.2%) was suspended in a mixture of methyl t-butyl ether (1300 ml) and DM water (400 ml). Aqueous sodium hydroxide solution (5 w/w; 133 g) was added to the suspended mass at 20-30° C. and stirred till clear solution was obtained. Thereafter, organic layer was separated and the aqueous layer was washed with methyl t-butyl ether. Thereafter, 20% aqueous ammonium formate solution (60 ml) was added and extracted with methylene chloride (300 ml). The organic layer was washed with DM water and concentrated under reduced pressure to yield a foamy mass. The concentrated mass was dissolved in ethylacetate (400 ml) and cooled to 0-5° C. To the solution, sodium ethoxide (10.77 g, mmol) was added and stirred at 20-30° C. for 90 min. The separated solid mass was filtered, washed with ethyl acetate and dried under reduced pressure at 40° C. to yield esomeprazole sodium.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08492551B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-f423ea6b9ac3460aa103689bf87e2690 |
|---|
| 出典メモ | uspto-grants-2013_07 |
|---|