Stavudine DMPU → Stavudine

HRID 913262

反応式

HRID 913262 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>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

3

反応物 1

HCID 86625622Stavudine DMPU

生成物 1

HCID 18283Stavudine収率 98.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

Stavudine DMPU solvate (25 g, 0.060 mole) is dissolved in isopropanol (250 ml), and treated with activated carbon anti-eno crowns (2.5 g) at reflux temperature. Reaction mass is filtered while hot and washed with hot isopropanol (25 ml). The combined filtrate and wash are concentrated to 100 ml and allowed the mass to cool to room temperature slowly. Cooled the mass to 0-5° C. and the precipitated product is filtered. washed the product with chilled isopropanol (10 ml) and air dried to give 13.2 g (83%) of the title compound which purity greater than 99%. XRD data resembles crystalline form-I

後処理

  1. additiontreated with activated carbon anti-eno crowns (2.5 g)
  2. temperatureat reflux temperature
  3. customReaction mass
  4. filtrationis filtered while hot and
  5. washwashed with hot isopropanol (25 ml)
  6. washThe combined filtrate and wash
  7. concentrationare concentrated to 100 ml
  8. temperatureCooled the mass to 0-5° C.
  9. filtrationthe precipitated product is filtered
  10. washwashed the product with chilled isopropanol (10 ml) and air
  11. customdried

出典と根拠

ORDレコード
ord-704beaa106dd4e47b01acf396000f4ad
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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