Diethylamine → Diethylamine

HRID 254882

반응식

HRID 254882 반응식
[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]

참가 물질

5

반응물 2

HCID 8021DiethylamineHCID 60823Atorvastatin3회

생성물 2

HCID 8021DiethylamineHCID 11556397Atorvastatin diethylamine

시약·촉매·용매 1

HCID 6342Acetonitrile용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a2c7032d7dd94e1b9535974ed076e7bf
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875731B2

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