化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Anhydride → Baccatin Iii
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 10-deacetylbaccatin III | HCID 154272 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 触媒 | Scandium(III) triflate | HCID 2734571 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Baccatin Iii | HCID 65366 | 58% |
| 生成物 | 10-deacetylbaccatin III | HCID 154272 | 18% |
反応手順
To a solution of 50 mg (91.9 μmol) of 10-deacetylbaccatin III and 13 μL (1.5 eq.) of acetic anhydride in 2.0 mL of freshly distilled tetrahydrofuran 100 μL of a solution of 4.5 mg of commercial scandium trifluoromethanesulfonate in 1.0 mL of tetrahydrofuran was added. The reaction mixture was stirred at room temperature for 48 hours. Usual workup and isolation of the product by means of preparative TLC (Silica 60, CH2Cl2/MeOH 10:1) afforded 9 mg of unreacted 10-deacetylbaccatin III (18%) along with 31 mg of baccatin III (58%). 1H-NMR and Rf-value (TLC) were in accordance with the product from example 1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05874595 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-8d7679915d9c41e98caf514da8929edb |
| 出典メモ | uspto-grants-1999_02 |