Water → Stavudine

HRID 913266

反応式

HRID 913266 の反応式
[CH3:1][C:2]1[C:8](=[O:9])[NH:7][C:5](=[O:6])[N:4]([C@@H:10]2[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]2)[CH:3]=1.CN1C(=O)N(C)CCC1.O>C(O)(C)C>[C@@H:10]1([N:4]2[CH:3]=[C:2]([CH3:1])[C:8](=[O:9])[NH:7][C:5]2=[O:6])[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]1

参加物

4

反応物 2

HCID 962WaterHCID 86625622HCID 86625622、化合物

生成物 1

HCID 18283Stavudine収率 88.6%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
2.5 °C

実験手順

Stavudine-DMPU solvate (25 g, 0.07 moles), water (5 g) and isopropanol (250 ml) are heated to about 82° C. to get clear colorless solution. Heating is continued so as to distill the solution at atmospheric pressure until about 80 ml of isopropanol remained in side. The solution is allowed to cool on its own. The mixture is further cooled to 0-5° C. for 1.5 hrs. The precipitated product is filtered, washed with isopropanol (2×10 ml) and air dried to give 13.9 g (87.2%) of pure white crystalline Stavudine. The HPLC results are given in Table 2.

後処理

  1. customto get clear colorless solution
  2. temperatureHeating
  3. distillationto distill the solution at atmospheric pressure until about 80 ml of isopropanol
  4. temperatureto cool on its own
  5. filtrationThe precipitated product is filtered
  6. washwashed with isopropanol (2×10 ml) and air
  7. customdried

出典と根拠

ORDレコード
ord-617fba8be3594a8fbcccd47e91e8e6a7
出典データセット
uspto-grants-2011_09
特許番号
US08026356B2

関連ノート

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