Monobenzone → 5-(p-Hydroxyphenoxy)pyrimidine

HRID 76130

反応式

HRID 76130 の反応式
[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

参加物

6

反応物 3

HCID 7638MonobenzoneHCID 10796Cesium carbonateHCID 783445-Bromopyrimidine

生成物 1

HCID 129406205-(p-Hydroxyphenoxy)pyrimidine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-e7978093a2dc4120954dbcd795fa8f7e
出典データセット
uspto-grants-2014_09
特許番号
US08835472B2

関連ノート

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