Stavudine → Stavudine DMA

HRID 988753

반응식

HRID 988753 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.[CH3:17][N:18]([CH3:22])[C:19](=[O:21])[CH3:20]>C(O)(C)C>[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.[CH3:20][C:19]([N:18]([CH3:22])[CH3:17])=[O:21]

참가 물질

4

반응물 2

HCID 18283StavudineHCID 31374Dimethylacetamide

생성물 1

HCID 11722976Stavudine DMA수율 75.2%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
79 °C

실험 절차

Crude slightly beige Stavudine (17.25 g, 96.02% pure, 0.0739 mole) was combined with N,N-dimethylacetamide (25.91 g, 1.5 parts) and isopropanol (52 mL, 3 volumes) and heated to 79° C. when all solids dissolved. The cloudy mixture was filtered through dicalite and washed with isopropanol (12.5 mL). The filtrate was initially concentrated at atmospheric pressure and then a slight vacuum was applied so that the distillation occurred at 60-70° C. It was estimated that about 1.7 g of isopropanol remained. The solution was cooled, filtered, washed and dried to give 17.30 g of Stavudine-DMA solvate (0.0556 mol, 75.2%) with a chromatographic purity of 99.59%.

후처리

  1. dissolutiondissolved
  2. filtrationThe cloudy mixture was filtered through dicalite
  3. washwashed with isopropanol (12.5 mL)
  4. concentrationThe filtrate was initially concentrated at atmospheric pressure
  5. distillationa slight vacuum was applied so that the distillation
  6. customoccurred at 60-70° C
  7. temperatureThe solution was cooled
  8. filtrationfiltered
  9. washwashed
  10. customdried

출처 및 근거

ORD 기록
ord-85d782a8316240bfb7eff0e710170867
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06635753B1

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