Water → Rosuvastatin

HRID 578743

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HRID 578743 반응식
[CH3:1][CH:2]([C:4]1[N:9]=[C:8]([N:10]([S:12]([CH3:15])(=[O:14])=[O:13])[CH3:11])[N:7]=[C:6]([C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)[C:5]=1/[CH:23]=[CH:24]/[C@@H:25]([OH:33])[CH2:26][C@@H:27]([OH:32])[CH2:28][C:29]([OH:31])=[O:30])[CH3:3].C([NH-])CCC.O.C(N)CCC>CC(O)C>[CH3:3][CH:2]([C:4]1[N:9]=[C:8]([N:10]([S:12]([CH3:15])(=[O:13])=[O:14])[CH3:11])[N:7]=[C:6]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[C:5]=1/[CH:23]=[CH:24]/[C@@H:25]([OH:33])[CH2:26][C@@H:27]([OH:32])[CH2:28][C:29]([OH:31])=[O:30])[CH3:1]

참가 물질

5

반응물 3

HCID 962WaterHCID 8007ButylamineHCID 86699893Rosuvastatin n-butylamide

생성물 1

HCID 446157Rosuvastatin수율 102.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
120 °C

실험 절차

An autoclave having 800 cm3 is charged with 16.1 g (0.03 mol) rosuvastatin n-butylamide, 644 cm3 of water and 43.9 g (63.3 cm3; 0.60 mol) of n-butylamine. The reaction mixture is stirred at 120° C. for 24 hours, allowed to cool, diluted with 2-propanol at room temperature and evaporated in vacuo. The residue is boiled in ethylacetate, and while stirring, allowed to cool to room temperature. The crystals are filtered. Thus 14.8 g (89%) of rosuvastatin NBA salt are obtained. The crude salt is stirred in ethylacetate at room temperature, filtered, washed and dried. Thus dried product is boiled in ethylacetate, thereafter stirred in the same solvent at room temperature, filtered, washed and dried. Yield 9.32 g (56%) of rosuvastatin NBA salt, having purity (as determined by HPLC) exceeding 99.5%.

후처리

  1. temperatureto cool
  2. customevaporated in vacuo
  3. stirringwhile stirring
  4. temperatureto cool to room temperature
  5. filtrationThe crystals are filtered

출처 및 근거

ORD 기록
ord-b9f9d6028af0454a98728bba3a69a714
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040696B2

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