Hydrogen Bromide → 2-Bromo-1-(2-phenyl-benzoxazol-6-yl)-butan-1-one

HRID 1619958노트

반응식

HRID 1619958 반응식
[C:1]1([C:7]2[O:8][C:9]3[CH:15]=[C:14]([C:16](=[O:20])[CH2:17][CH2:18][CH3:19])[CH:13]=[CH:12][C:10]=3[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br-:21].[Br-].[Br-].[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1.Br.C(=O)([O-])[O-].[K+].[K+]>C(O)(=O)C.O>[Br:21][CH:17]([CH2:18][CH3:19])[C:16]([C:14]1[CH:13]=[CH:12][C:10]2[N:11]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[O:8][C:9]=2[CH:15]=1)=[O:20]

참가 물질

7

반응물 4

HCID 260Hydrogen BromideHCID 11430Potassium CarbonateHCID 21124087PyridiniumtribromideHCID 674660111-(2-Phenyl-benzoxazol-6-yl)butan-1-one

생성물 1

HCID 866890652-Bromo-1-(2-phenyl-benzoxazol-6-yl)-butan-1-one

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매

실험 절차

400 mg (1.51 mmol) 1-(2-phenyl-benzoxazol-6-yl)-butan-1-one and 643 mg (1.81 mmol) pyridinium tribromide are dissolved in 4 ml glacial acetic acid at RT, then 1.04 ml (5.40 mmol) hydrogen bromide, dissolved 30% in glacial acetic acid, are added and the mixture is stirred for 1 h at RT. Then the reaction mixture is mixed with water and adjusted to pH 8 with 5% potassium carbonate solution, then it is extracted with DCM, the org. phase is dried on magnesium sulphate and the solv. is eliminated completely in vacuo. The residue is separated through silica gel (eluant cyclohexane/EA).

후처리

  1. additionare added
  2. extractionit is extracted with DCM
  3. customphase is dried on magnesium sulphate
  4. customThe residue is separated through silica gel (eluant cyclohexane/EA)

출처 및 근거

ORD 기록
ord-2aff2ccdaab2469fa39985af4e4f2357
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772323B2

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