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Potassium Phosphate, Tribasic → (R)-1-[4-(4-chlorophenoxy)phenyl]-5-[3-(trifluoromethyl)phenyl]pyrrolidin-2-one

HRID 1972239
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HRID 1972239 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([C@@H:9]2[NH:13][C:12](=[O:14])[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.I[C:18]1[CH:31]=[CH:30][C:21]([O:22][C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=2)=[CH:20][CH:19]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([O:22][C:21]2[CH:30]=[CH:31][C:18]([N:13]3[C@@H:9]([C:5]4[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:4]=4)[CH2:10][CH2:11][C:12]3=[O:14])=[CH:19][CH:20]=2)=[CH:24][CH:25]=1
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6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 193519904-(4-Chlorophenoxy)iodobenzeneHCID 59485901(R)-5-[3-(trifluoromethyl)phenyl]pyrrolidin-2-one

생성물 1

HCID 59485681(R)-1-[4-(4-chlorophenoxy)phenyl]-5-[3-(trifluoromethyl)phenyl]pyrrolidin-2-one

시약·촉매·용매 2

HCID 83717Copper iodide촉매
HCID 31275
1,4-Dioxane
용매

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온도
110 °C

실험 절차

To a 10 mL reaction tube fitted with a screw cap is charged with (R)-5-[3-(trifluoromethyl)phenyl]pyrrolidin-2-one (90 mg, 0.39 mmol) and 1,4-dioxane (3 mL). 1-(4-iodophenoxy)-4-chlorobenzene (157 mg, 0.47 mmol) is then added, followed by copper iodide (15 mg, 0.078 mmol), N,N′-1,2-trans-dimethylcyclohexane-1,2-diamine (11.2 mg, 0.078 mmol), and K3PO4 (167 mg, 0.78 mmol). The system is degassed with argon then sealed and heated to 110° C. for 28 h. The reaction is cooled to room temperature, dissolved in ethyl acetate and washed with water and brine. The organic phase is dried over Na2SO4, filtered and concentrated in vacuo. Purification on silica gel (0-30% ethyl acetate in hexane) gave (R)-1-[4-(4-chlorophenoxy)phenyl]-5-[3-(trifluoromethyl)phenyl]pyrrolidin-2-one as a slightly yellow oil (102 mg, 60%). 1H NMR (CDCl3) δ (ppm) 7.60-7.50 (m, 1H), 7.49-7.37 (m, 3H), 7.34-7.28 (m, 2H), 7.27-7.21 (m, 2H), 6.91-6.67 (m, 4H), 5.28 (dd, J=6.8, 5.6 Hz, 1H), 2.84-2.59 (m, 3H), 2.07-1.94 (m, 1H). HPLC-MS calculated for C23H17ClF3NO2 (M+H+) 432.09, found 432.10.

후처리

  1. customTo a 10 mL reaction tube
  2. customfitted with a screw
  3. customcap
  4. customThe system is degassed with argon
  5. customthen sealed
  6. temperatureThe reaction is cooled to room temperature
  7. dissolutiondissolved in ethyl acetate
  8. washwashed with water and brine
  9. dry with materialThe organic phase is dried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo
  12. customPurification on silica gel (0-30% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-8818ccb6a96747ce913d46714a581edf
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08431607B2

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