Benzoyl Peroxide → 2-(3-{[Tert-butyl-(dimethyl)silyl]oxy}-4-bromomethylphenyl)-1,3-benzoxazole

HRID 7710

반응식

HRID 7710 반응식
[C:1]([Si:5]([CH3:24])([CH3:23])[O:6][C:7]1[CH:8]=[C:9]([C:14]2[O:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[N:18]=2)[CH:10]=[CH:11][C:12]=1[CH3:13])([CH3:4])([CH3:3])[CH3:2].C1C(=O)N([Br:32])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[C:1]([Si:5]([CH3:24])([CH3:23])[O:6][C:7]1[CH:8]=[C:9]([C:14]2[O:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[N:18]=2)[CH:10]=[CH:11][C:12]=1[CH2:13][Br:32])([CH3:2])([CH3:4])[CH3:3]

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 695845442-(3-{[Tert-butyl-(dimethyl)silyl]oxy}-4-methylphenyl)-1,3-benzoxazole

생성물 1

HCID 695845532-(3-{[Tert-butyl-(dimethyl)silyl]oxy}-4-bromomethylphenyl)-1,3-benzoxazole

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To 2-(3-{[tert-butyl-(dimethyl)silyl]oxy}-4-methylphenyl)-1,3-benzoxazole (1.46 g, 4.3 mmol) in CCl4 (50 mL) was added NBS (770 mg, 4.3 mmol) and benzoyl peroxide (50 mg). The reaction mixture was refluxed for 6 h, cooled to rt, and CCl4 was removed in vacuo. The residue was dissolved in EtOAc (50 mL), washed with H2O (50 mL), dried (MgSO4), filtered and concentrated in vacuo to afford 2-(3-{[tert-butyl-(dimethyl)silyl]oxy}-4-bromomethylphenyl)-1,3-benzoxazole as light yellow solid.

후처리

  1. temperatureThe reaction mixture was refluxed for 6 h
  2. customCCl4 was removed in vacuo
  3. dissolutionThe residue was dissolved in EtOAc (50 mL)
  4. washwashed with H2O (50 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f439900152384de1b2022bdb92a51c52
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087601B2

연결된 노트

불러오는 중…