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Chlorotrimethylsilane → 5-[2-Benzyloxy-4-(6-benzyloxypyridin-2-ylmethyl)-phenyl]-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one

HRID 660544
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인쇄 미리보기

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HRID 660544 반응식
BrCCBr.C[Si](Cl)(C)C.[CH2:10]([O:17][C:18]1[CH:23]=[C:22]([CH2:24]I)[CH:21]=[CH:20][C:19]=1[N:26]1[S:30](=[O:32])(=[O:31])[N:29]([CH2:33][CH2:34][Si:35]([CH3:38])([CH3:37])[CH3:36])[C:28](=[O:39])[CH2:27]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C1(C2C=CC=CC=2)C=CC=CC=1.[CH2:52]([O:59][C:60]1[CH:65]=[CH:64][CH:63]=[C:62](Br)[N:61]=1)[C:53]1[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=1>CN(C)C(=O)C.[Zn].C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH2:10]([O:17][C:18]1[CH:23]=[C:22]([CH2:24][C:62]2[CH:63]=[CH:64][CH:65]=[C:60]([O:59][CH2:52][C:53]3[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=3)[N:61]=2)[CH:21]=[CH:20][C:19]=1[N:26]1[S:30](=[O:32])(=[O:31])[N:29]([CH2:33][CH2:34][Si:35]([CH3:38])([CH3:37])[CH3:36])[C:28](=[O:39])[CH2:27]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 6397ChlorotrimethylsilaneHCID 7095BiphenylHCID 78391,2-DibromoethaneHCID 8174752-Benzyloxy-6-bromopyridineHCID 667568095-(2-Benzyloxy-4-iodomethylphenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one

생성물 1

HCID 68838834
5-[2-Benzyloxy-4-(6-benzyloxypyridin-2-ylmethyl)-phenyl]-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one

시약·촉매·용매 3

HCID 23994Zinc촉매2회HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 31374Dimethylacetamide용매3회

실험 절차

In a pressure vessel, zinc powder (429 mg, 6.6 mmol) is dried by heating under vacuum, then cooled, placed under N2, and slurried in N,N-dimethylacetamide (0.75 mL). To the slurry is added 1,2-dibromoethane (0.044 mL, 0.51 mmol) and the mixture is heated until boiling. The mixture is allowed to cool, and TMSCl (65 mL, 0.51 mmol) is added, followed by stirring for 30 min to produce a green solution. To the activated zinc is added 5-(2-benzyloxy-4-iodomethylphenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one (600 mg, 1.1 mmol) in N,N-dimethylacetamide (1 mL) over 30 min. The organozinc solution is filtered and degassed with N2, then to it is added Pd2(dba)3 (50 mg, 0.055 mmol) and 2-di-t-butylphosphino)biphenyl (66 mg, 0.22 mmol), followed by degassed 2-benzyloxy-6-bromopyridine (350 mg, 1.3 mmol) in N,N-dimethylacetamide. The vessel is sealed and the reaction is stirred at 80° C. for 18 h. The reaction is allowed to cool to RT then is filtered through Celite. The resulting solution is diluted with EtOAc (10 mL) and washed with water and brine, then dried over MgSO4. The solvent is removed under reduced pressure and the crude residue is purified by silica gel chromatography using a gradient of 0-75% EtOAc/hexane to afford the title compound as a colorless oil: (M+H)+=616

후처리

  1. temperatureby heating under vacuum
  2. temperaturecooled
  3. temperaturethe mixture is heated until boiling
  4. temperatureto cool
  5. customto produce a green solution
  6. filtrationThe organozinc solution is filtered
  7. customdegassed with N2
  8. customThe vessel is sealed
  9. stirringthe reaction is stirred at 80° C. for 18 h
  10. filtrationthen is filtered through Celite
  11. additionThe resulting solution is diluted with EtOAc (10 mL)
  12. washwashed with water and brine
  13. dry with materialdried over MgSO4
  14. customThe solvent is removed under reduced pressure
  15. customthe crude residue is purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-846673c26e664899b472e1c0d502d6f6
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084448B2

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