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Azobisisobutyronitrile → 6-(Bromomethyl)benzo[d]oxazole

HRID 1004317
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인쇄 미리보기

반응식

HRID 1004317 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][O:8][C:4]=2[CH:3]=1.[Br:11]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)Cl>[Br:11][CH2:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][O:8][C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 27249696-Methylbenzoxazole

생성물 1

HCID 219850576-(Bromomethyl)benzo[d]oxazole수율 77.9%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 6-methylbenzoxazole (5.0 g; J. T. Gupton, K. F. Correia and B. S. Foster, Synthetic Communications, 1986, 16, 365), N-bromosuccinimide (7.0 g) and azobisisobutyronitrile (0.55 g) in dry chloroform (100 ml) was heated at reflux for 1 hour. The cooled reaction mixture was washed three times with water (40 ml), dried over magnesium sulphate and evaporated. The residual orange coloured viscous solid was triturated twice with pentane (50 ml) affording the title compound (6.20 g) as a buff coloured solid, m.p. 52-56° C.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 1 hour
  3. customThe cooled reaction mixture
  4. washwas washed three times with water (40 ml)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customwas triturated twice with pentane (50 ml)

출처 및 근거

ORD 기록
ord-73ba69673ea74b60b537ac0003fae1a0
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06048893

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