Diethylamine → Diethylamine

HRID 254882

反応式

HRID 254882 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[CH3:6][CH:7]([C:9]1[N:13]([CH2:14][CH2:15][C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([OH:22])=[O:21])[C:12]([C:25]2[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=2)=[C:11]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:10]=1[C:38]([NH:40][C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)=[O:39])[CH3:8]>C(#N)C>[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[CH3:8][CH:7]([C:9]1[N:13]([CH2:14][CH2:15][C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([OH:22])=[O:21])[C:12]([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[C:11]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:10]=1[C:38]([NH:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:39])[CH3:6].[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2]

参加物

5

反応物 2

HCID 8021DiethylamineHCID 60823Atorvastatin3 回

生成物 2

HCID 8021DiethylamineHCID 11556397Atorvastatin diethylamine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒3 回

実験手順

The diethylamine 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 diethylamine was prepared by dissolving 132.33 mg (1.0 equivalents) in acetonitrile (20 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 diethylamine 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-a2c7032d7dd94e1b9535974ed076e7bf
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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