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Oxalic Acid → (2,4-Difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxalate

HRID 55630
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HRID 55630 반응식
C(O[C:4]([CH:6]1[CH2:10][CH2:9][N:8]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:7]1)=[O:5])C.S(Cl)(Cl)=O.[F:22][C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([F:29])[CH:24]=1.[Cl-].[Al+3].[Cl-].[Cl-].[C:34]([OH:39])(=[O:38])[C:35]([OH:37])=[O:36]>Cl.C(O)C.CCOCC>[C:34]([OH:39])(=[O:38])[C:35]([OH:37])=[O:36].[F:22][C:23]1[CH:24]=[C:25]([F:29])[CH:26]=[CH:27][C:28]=1[C:4]([CH:6]1[CH2:10][CH2:9][N:8]([CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:7]1)=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 971Oxalic AcidHCID 97411,3-DifluorobenzeneHCID 24386Thionyl ChlorideHCID 6451240Aluminum(III) ChlorideHCID 11622765Ethyl 1-benzylpyrrolidine-3-carboxylate

생성물 1

HCID 21960052(2,4-Difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxalate수율 57.4%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매2회HCID 3283Diethyl Ether용매

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온도
55 °C

실험 절차

In a 1 liter round bottom flask, a solution of ethyl-N-benzyl-3-pyrrolidine carboxylate (21.8 g, 11.7 mmol) in 140 ml of 6N HCl was heated at reflux for 2.5 hours. The solution was cooled and the solvent was removed to dryness with a vacuum pump. The residue was then treated with thionyl chloride (100 ml) for 16 hours at room temperature. After the reaction, the excess thionyl chloride was vacuum stripped to dryness (60° C., 4 hours). To the residue in the flask was added 1,3-difluorobenzene (30 g, 26 mmol) followed by aluminum chloride (25 g, 18.7 mmol) in portions at room temperature. When the mixture turned homogeneous (in about 10 minutes) it was then heated at 55° C. for 1 hour. After the reaction was complete, excess 1,3-difluorobenzene was removed under reduced pressure. The residue was partitioned between ice/water and dichloromethane (700 ml) and basified with 50% NaOH solution to pH 10. The dichloromethane solution was washed with water and brine, then dried over anhydrous MgSO4. The solvent was stripped and the crude oil (31 g) was purified by flash chromatography over a silica gel column. The pure product thus obtained weighed 26 g (74%) as a yellow oil. An analytical sample was prepared by dissolving 4.2 g of the oil in ethanol and treating with an ethanol solution of oxalic acid (1.33 g, 14.8 mmol). To the mixture was added ether dropwise to cause crystallization. Recrystallization from ethanol and ether gave 2.63 g of (2,4-difluorophenyl)[1-(phenylmethyl)-3-pyrrolidinyl]methanone oxalate as white crystals, m.p.=114°-116° C.

후처리

  1. temperatureat reflux for 2.5 hours
  2. temperatureThe solution was cooled
  3. customthe solvent was removed to dryness with a vacuum pump
  4. additionThe residue was then treated with thionyl chloride (100 ml) for 16 hours at room temperature
  5. customAfter the reaction
  6. customstripped to dryness (60° C., 4 hours)
  7. custom(in about 10 minutes) it
  8. customexcess 1,3-difluorobenzene was removed under reduced pressure
  9. customThe residue was partitioned between ice/water and dichloromethane (700 ml)
  10. washThe dichloromethane solution was washed with water and brine
  11. dry with materialdried over anhydrous MgSO4
  12. customthe crude oil (31 g) was purified by flash chromatography over a silica gel column
  13. customThe pure product thus obtained
  14. customAn analytical sample was prepared
  15. customcrystallization
  16. customRecrystallization from ethanol and ether

출처 및 근거

ORD 기록
ord-722d7d18effd4c0fb45aca8c2d71655a
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05624927

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