Heptane → Montelukast sodium

HRID 1931356

반응식

HRID 1931356 반응식
[CH3:1][C:2]([OH:41])([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:9]=1[CH2:10][CH2:11][C@@H:12]([S:32][CH2:33][C:34]1([CH2:37][C:38]([OH:40])=[O:39])[CH2:36][CH2:35]1)[C:13]1[CH:14]=[CH:15][CH:16]=[C:17](/[CH:19]=[CH:20]/[C:21]2[CH:22]=[CH:23][C:24]3[CH:25]=[CH:26][C:27]([Cl:31])=[CH:28][C:29]=3[N:30]=2)[CH:18]=1)[CH3:3].[OH-].[Na+:43].CCCCCCC>C1(C)C=CC=CC=1.CO.C(OCC)(=O)C>[CH3:3][C:2]([OH:41])([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:9]=1[CH2:10][CH2:11][C@@H:12]([S:32][CH2:33][C:34]1([CH2:37][C:38]([O-:40])=[O:39])[CH2:35][CH2:36]1)[C:13]1[CH:14]=[CH:15][CH:16]=[C:17](/[CH:19]=[CH:20]/[C:21]2[CH:22]=[CH:23][C:24]3[CH:25]=[CH:26][C:27]([Cl:31])=[CH:28][C:29]=3[N:30]=2)[CH:18]=1)[CH3:1].[Na+:43]

참가 물질

7

반응물 3

HCID 8900HeptaneHCID 14798Sodium HydroxideHCID 5281040Montelukast

생성물 1

HCID 23663996Montelukast sodium수율 100%

시약·촉매·용매 3

HCID 887Methanol용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

2.6 g of Montelukast acid were dissolved in 26 ml of toluene and 8.9 ml of 0.5M NaOH solution in methanol were added slowly at room temperature. The mixture was stirred for 1 hour and the solvent was removed under vacuum to obtain a residue. Then, heptane (24 ml) was added over 30 minutes to a well stirred solution of the residue in 4 ml of ethyl acetate at room temperature. Two hours after the addition, an off white solid was filtered off under a nitrogen atmosphere and washed with 5 ml of heptane. The wet product was dried under vacuum at 70-80° C. for 2 days to yield 2.7 g of Montelukast sodium. Yield: 100%.

후처리

  1. customthe solvent was removed under vacuum
  2. customto obtain a residue
  3. additionTwo hours after the addition
  4. filtrationan off white solid was filtered off under a nitrogen atmosphere
  5. washwashed with 5 ml of heptane
  6. customThe wet product was dried under vacuum at 70-80° C. for 2 days

출처 및 근거

ORD 기록
ord-7454bdd2f0f045a8b75482ae37384ee9
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188285B2

연결된 노트

불러오는 중…