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Dimethyl Sulfate → Methyldigoxin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Digoxin | HCID 2724385 | — |
| 反応物 | Strontium hydroxide octahydrate | HCID 21617461 | — |
| 生成物 | Methyldigoxin | HCID 443946 | 72.62% |
| 生成物 | Digoxin | HCID 2724385 | 17.16% |
反応手順
A solution of 2.34 g (3 millimoles) of digoxin is treated with 797 mg (3 millimoles) of strontium hydroxide octahydrate and the mixture is methylated with 757 g (6 millimoles) of dimethyl sulfate at 0° C., the procedure being the same as in Example 6. Evaporation of the fractions collected gives 119 mg (4.90% of theory of dimethyldigoxin, 403 mg (17.16%) of digoxin and 1.732 g (72.62% of theory) of β-methyldigoxin, from which 1.59 g of pure β-methyldigoxin are obtained after recrystallization from acetone. The yield is 66.67% and the selectivity of the reaction is 80.48%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04603196 |
| 出典データセット | uspto-grants-1986_07 |
| ORD ID | ord-f88a971728074acd92bfd58f34c6e99b |
| 出典メモ | uspto-grants-1986_07 |