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Sodium Sulfate → 6-{[(3R)-1-benzyl-3-pyrrolidinyl]amino}-5-fluoronicotinaldehyde

HRID 2376146
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HRID 2376146 반응식
[H-].C([Al+]CC(C)C)C(C)C.[CH2:11]([N:18]1[CH2:22][CH2:21][C@@H:20]([NH:23][C:24]2[C:34]([F:35])=[CH:33][C:27]([C:28](OCC)=[O:29])=[CH:26][N:25]=2)[CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-].[NH4+].[O-]S([O-])(=O)=O.[Na+].[Na+]>CCCCCC.C1COCC1>[CH2:11]([N:18]1[CH2:22][CH2:21][C@@H:20]([NH:23][C:24]2[C:34]([F:35])=[CH:33][C:27]([CH:28]=[O:29])=[CH:26][N:25]=2)[CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 24436Sodium SulfateHCID 25517Ammonium ChlorideHCID 21225700DiisobutylaluminumhydrideHCID 68963376ethyl 6-{[(3R)-1-benzyl-3-pyrrolidinyl]amino}-5-fluoronicotinate

생성물 1

HCID 866037566-{[(3R)-1-benzyl-3-pyrrolidinyl]amino}-5-fluoronicotinaldehyde수율 98%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8058Hexane용매

실험 절차

0.94 M solution of diisobutylaluminium hydride in hexane (2.73 ml) was added dropwise to a solution of ethyl 6-{[(3R)-1-benzyl-3-pyrrolidinyl]amino}-5-fluoronicotinate (294 mg) in THF (10 ml) with stirred below 5° C. under atmospheric pressure of nitrogen, and the reaction mixture was stirred at the same temperature for 1.5 hrs. To the reaction mixture was added saturated aqueous ammonium chloride (0.727 ml) below 5° C., then the mixture was stirred at 25° C. for 30 minutes. Na2SO4 (2.87 g) was added to the solution, and the mixture was stirred at 25° C. for 15 minutes. The reaction mixture was filtrated, the filtrate was evaporated in vacuo. Toluene (15 ml) was added to the residue, and the mixture was evaporated in vacuo. The resulting residue and activated MnO2 (744 mg) in ethyl, acetate (20 ml) were stirred at 75° C. for 1 hour. After removal of the insoluble material by filtration, the filtrate was evaporated in vacuo to give 6-{[(3R)-1-benzyl-3-pyrrolidinyl]amino}-5-fluoronicotinaldehyde (250 mg, 98%) as syrup. The compound was used in the next step reaction without purification.

후처리

  1. stirringthe reaction mixture was stirred at the same temperature for 1.5 hrs
  2. stirringthe mixture was stirred at 25° C. for 30 minutes
  3. stirringthe mixture was stirred at 25° C. for 15 minutes
  4. filtrationThe reaction mixture was filtrated
  5. customthe filtrate was evaporated in vacuo
  6. additionToluene (15 ml) was added to the residue
  7. customthe mixture was evaporated in vacuo
  8. stirringThe resulting residue and activated MnO2 (744 mg) in ethyl, acetate (20 ml) were stirred at 75° C. for 1 hour
  9. customAfter removal of the insoluble material
  10. filtrationby filtration
  11. customthe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-253a5bb080d744fe8cbe549786217edb
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07465731B2

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