Water → Rosuvastatin

HRID 578743

反応式

HRID 578743 の反応式
[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]

参加物

5

反応物 3

HCID 962WaterHCID 8007ButylamineHCID 86699893Rosuvastatin n-butylamide

生成物 1

HCID 446157Rosuvastatin収率 102.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
120 °C

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-b9f9d6028af0454a98728bba3a69a714
出典データセット
uspto-grants-2015_05
特許番号
US09040696B2

関連ノート

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