関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Gemcitabine | HCID 60750 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Gemcitabine Hydrochloride | HCID 60749 | — |
反応手順
To the 20 g of thick oil of Gemcitabine base obtained as in example 3 was added 1,4-Dioxane (120 ml) and the mixture was heated to 60°-68° C. and stirred for 15 minutes. Conc. HCl (10 ml) was then added to the mixture and the contents were heated at same temperature for one hour. Reaction mass was then cooled to 10-15° C. and maintained for 30 minutes. The solid thus obtained was filtered off and washed with 1,4-Dioxane and dried under vacuum at 55-60° C. to get 8 g material with Specific Optical Rotation i.e.[α]D=+40° and HPLC purity of 85% β-anomer and 8% α-anomer.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08193354B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-e4b3723cf41e44089ee9b2568a14a59f |
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| 出典メモ | uspto-grants-2012_06 |
|---|