Monobenzone → 5-(p-Hydroxyphenoxy)pyrimidine

HRID 76130

반응식

HRID 76130 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1C=CC=CC=1.BrC1[CH:18]=[N:19][CH:20]=[N:21]C=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.O>[OH:15][C:12]1[CH:11]=[CH:10][C:9]([O:8][C:1]2[CH:2]=[N:21][CH:20]=[N:19][CH:18]=2)=[CH:14][CH:13]=1

참가 물질

6

반응물 3

HCID 7638MonobenzoneHCID 10796Cesium carbonateHCID 783445-Bromopyrimidine

생성물 1

HCID 129406205-(p-Hydroxyphenoxy)pyrimidine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

To 1.00 g (4.99 mmol) 4-(benzyloxy)phenol and 794 mg (4.99 mmol) 5-bromo-pyrimidine in 5 mL DMF are added 3.25 g (9.99 mmol) Cs2CO3 and the reaction mixture is stirred at 120° C. for 6 h in a microwave oven. Then the reaction mixture is diluted with water and extracted with EtOAc. The organic layer is dried with Na2SO4 and the solvent is removed in vacuo. The residue is purified by HPLC (MeOH/H2O/NH3).

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe organic layer is dried with Na2SO4
  3. customthe solvent is removed in vacuo
  4. customThe residue is purified by HPLC (MeOH/H2O/NH3)

출처 및 근거

ORD 기록
ord-e7978093a2dc4120954dbcd795fa8f7e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835472B2

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