Acetonitrile → Benzathine

HRID 71011

반응식

HRID 71011 반응식
[CH3:1][CH:2]([C:4]1[N:8]([CH2:9][CH2:10][C@@H:11]([OH:19])[CH2:12][C@@H:13]([OH:18])[CH2:14][C:15]([OH:17])=[O:16])[C:7]([C:20]2[CH:21]=[CH:22][C:23]([F:26])=[CH:24][CH:25]=2)=[C:6]([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:5]=1[C:33]([NH:35][C:36]1[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=1)=[O:34])[CH3:3].[C:42](#[N:44])[CH3:43]>O>[CH:4]1[CH:5]=[CH:6][C:43]([CH2:42][NH:44][CH2:10][CH2:9][NH:8][CH2:7][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:1][CH:2]=1.[CH3:3][CH:2]([C:4]1[N:8]([CH2:9][CH2:10][C@@H:11]([OH:19])[CH2:12][C@@H:13]([OH:18])[CH2:14][C:15]([OH:17])=[O:16])[C:7]([C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)=[C:6]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:5]=1[C:33]([NH:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:34])[CH3:1].[C:27]1([CH2:6][CH:7]([NH2:8])[CH2:20][NH2:44])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

참가 물질

6

반응물 2

HCID 6342Acetonitrile2회HCID 60823Atorvastatin2회

생성물 3

HCID 8793BenzathineHCID 60823AtorvastatinHCID 4134343-Phenylpropane-1,2-diamine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The benzathine salt of atorvastatin (Form B) 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,N′-bis(phenylmethyl-1,2-ethanediamine (benzathine) was prepared by dissolving 220.64 mg (0.5 equivalents) in acetonitrile (80 mL) and water (20 mL). The stock solution of atorvastatin free acid was added to the counterion solution with stirring. After 2 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) to afford atorvastatin benzathine Form B. Note that this procedure is the same as above except that the sample was not oven dried.

후처리

  1. stirringAfter 2 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)

출처 및 근거

ORD 기록
ord-45777a62c3a540f0aec199c98e0a898a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822703B2

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