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Dichloromethane → Rocuronium Bromide Impurity 31
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 反応物 | 2beta-(4-Morpholinyl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol | HCID 16063873 | — |
| 生成物 | Rocuronium Bromide Impurity 31 | HCID 54054638 | — |
反応手順
Acetyl chloride (10.0 ml) was added to a stirred suspension of (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol (10.0 g) in dichloromethane (100 ml). After 24 h. at room temperature, saturated potassium bicarbonate solution (approx. 20 ml) was added to give pH>7; the dichloromethane layer was separated, washed with water (3×150 ml), dried (Na2SO4) and evaporated to dryness to afford (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol diacetate as an off-white froth (7.78 g), [α]D20 =+11.4° (c 0.57 in CHCl3)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04894369 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-c5a64f943f3e4db88c7d98b09311a238 |
| 出典メモ | uspto-grants-1990_01 |