Atorvastatin → N-Benzylphenethylamine

HRID 254878

反応式

HRID 254878 の反応式
CC(C1[N:8]([CH2:9][CH2:10][C@@H:11](O)[CH2:12][C@@H:13](O)[CH2:14][C:15](O)=O)[C:7](C2C=CC(F)=CC=2)=[C:6]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)C=1C(NC1C=CC=CC=1)=O)C>C(#N)C>[CH2:9]([NH:8][CH2:7][CH2:6][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

参加物

3

反応物 1

HCID 60823Atorvastatin3 回

生成物 1

HCID 65055N-Benzylphenethylamine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒3 回

実験手順

The benethamine salt of atorvastatin (Form A) was synthesized by preparing a stock solution of the free acid of atorvastatin (U.S. Pat. No. 5,273,995) in acetonitrile (1 g in 40 mL of ACN). A solution of N-benzyl-2-phenylethylamine (benethamine) was prepared by dissolving 378.59 mg (1.0 equivalents) in acetonitrile (10 mL). The stock solution of atorvastatin free acid was added to the counterion solution with stirring. Over time, an additional 40 mL of acetonitrile was added to prevent the formation of a gel. After 5 days of stirring at ambient temperature, the solids were isolated by vacuum filtration using a Buchner funnel fitted with a paper filter (#2 Whatman). The solids were rinsed with acetonitrile (75 mL), and placed in a 25° C. oven under nitrogen to dry overnight to afford atorvastatin benethamine Form A.

後処理

  1. stirringAfter 5 days of stirring at ambient temperature
  2. customthe solids were isolated by vacuum filtration
  3. customfitted with a paper
  4. filtrationfilter (#2 Whatman)
  5. washThe solids were rinsed with acetonitrile (75 mL)
  6. customplaced in a 25° C.
  7. customto dry overnight

出典と根拠

ORDレコード
ord-080833ed0c6b4b40b57e03ae3fdc765f
出典データセット
uspto-grants-2011_01
特許番号
US07875731B2

関連ノート

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