Stavudine DMPU → Stavudine

HRID 913262

반응식

HRID 913262 반응식
[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

참가 물질

3

반응물 1

HCID 86625622Stavudine DMPU

생성물 1

HCID 18283Stavudine수율 98.1%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-704beaa106dd4e47b01acf396000f4ad
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026356B2

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