化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → HCID 178488147、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Esomeprazole BINOL | HCID 178488158 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | HCID 178488147 | HCID 178488147 | — |
反応手順
Esomeprazole-BINOL inclusion complex (100 g; 158.29 mmol; ee of 98.28%) was suspended in methyl t-butyl ether (1300 ml). Aqueous sodium hydroxide solution (2.2% w/w; 302 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 extracted with methyl t-butyl ether for recovery of BINOL. The organic layers were combined, concentrated and recovered 44.4 g of BINOL. To the aqueous layer, methylene chloride (300 ml) was added and pH was adjusted to 7-8 with 10% v/v aqueous acetic acid. The organic layer was separated and washed with DM water and concentrated under reduced pressure to yield esomeprazole as a foamy solid mass.
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-cde4a1f00bf740c79c04cb230bec1eb0 |
| 出典メモ | uspto-grants-2013_07 |