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Iodobenzene → 2-Phenethyl-1,4-bis-(toluene-4-sulfonyl)-piperazine

HRID 1350381
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HRID 1350381 반응식
B1[CH:6]2[CH2:7][CH2:8][CH2:9][CH:2]1CC[CH2:5]2.[C:10]1([CH3:37])[CH:15]=[CH:14][C:13]([S:16]([N:19]2[CH2:24][CH2:23][N:22]([S:25]([C:28]3[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=3)(=[O:27])=[O:26])[CH2:21][C@@H:20]2[CH:35]=[CH2:36])(=[O:18])=[O:17])=[CH:12][CH:11]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.IC1C=CC=CC=1.[OH-].[Na+]>C1COCC1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH2:35]([CH:20]1[CH2:21][N:22]([S:25]([C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)(=[O:27])=[O:26])[CH2:23][CH2:24][N:19]1[S:16]([C:13]1[CH:14]=[CH:15][C:10]([CH3:37])=[CH:11][CH:12]=1)(=[O:17])=[O:18])[CH2:36][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 11575IodobenzeneHCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 789669-Borabicyclo(3.3.1)nonaneHCID 14612246(S)-1,4-bis(toluene-4-sulfonyl)-2-vinyl-piperazine

생성물 1

HCID 694865562-Phenethyl-1,4-bis-(toluene-4-sulfonyl)-piperazine수율 75%

시약·촉매·용매 2

HCID 11979704Tetrakis(triphenylphosphine)palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

Add 9-BBN (0.5 M THF solution, 13.7 mL, 6.85 mmol) to a 100 mL schlenk flask containing (S)-1,4-bis(toluene-4-sulfonyl)-2-vinyl-piperazine(0.96 g, 2.3 mmol) in THF (5 mL), at room temperature under nitrogen and stir. After 18 hours, treat the reaction with tetrakis(triphenylphosphine) palladium (53 mg, 0.046 mmol), triphenyl phosphine (94.6 mg, 0.36 mmol), iodiobenzene (0.703 g, 3.4 mmol) and 3N NaOH (2.8 mL, 8.4 mmol) and heat to reflux. After 24 hours, cool the reaction to room temperature, remove in vacuo the THF solvent, dilute the residue with CH2Cl2, wash with 1N HCl, brine, and dry over Na2SO4. Purification by flash chromatography twice (Gradient: Hexanes/CH2Cl2=50/50, to Hexanes/CH2Cl2/EtOAc=40/40/10), and recrystallization in MeOH gives 860 mg (75%) of the title compound: mass spectrum (electrospray): (m/z)=499.2 (M+1); 1H NMR (CDCl3): δ7.58–7.54 (m, 4H), 7.33–7.20 (m, 7H), 7.19–7.07 (m, 2H), 3.99 (m, 1H), 3.81–3.78 (m, 1H), 3.64–3.60 (m, 2H), 3.22 (dt, 1H, J=3.2 Hz, J=12.4 Hz), 2.57–2.41 (m, 2H), 2.41 (s, 3H), 2.33 (s, 3H), 2.33–2.20 (m, 2H), 2.03–1.98 (m, 1H), 1.75–1.63 (m, 1H).

후처리

  1. additiontreat
  2. temperatureheat to reflux
  3. waitAfter 24 hours
  4. temperaturecool
  5. customthe reaction to room temperature
  6. customremove in vacuo the THF solvent
  7. additiondilute the residue with CH2Cl2
  8. washwash with 1N HCl, brine
  9. dry with materialdry over Na2SO4
  10. customPurification
  11. customby flash chromatography twice (Gradient: Hexanes/CH2Cl2=50/50, to Hexanes/CH2Cl2/EtOAc=40/40/10), and recrystallization in MeOH

출처 및 근거

ORD 기록
ord-a1f9ab8ea5f44ab892ea2e5898ea6d0a
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214673B2

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