Boron tribromide → 5-(p-Hydroxyphenoxy)pyrimidine

HRID 1413052

反応式

HRID 1413052 の反応式
C[O:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][C:8]2[CH:9]=[N:10][CH:11]=[N:12][CH:13]=2)=[CH:5][CH:4]=1.B(Br)(Br)Br>ClCCl>[OH:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][C:8]2[CH:13]=[N:12][CH:11]=[N:10][CH:9]=2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 20292632HCID 20292632、化合物

生成物 1

HCID 129406205-(p-Hydroxyphenoxy)pyrimidine収率 5.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5-(p-Methoxyphenoxy)pyrimidine (7.7 g) was dissolved in dichloromethane and the solution, maintained at a temperature of -70° to -78° C., was treated by the dropwise addition of boron tribromide (7 ml). The stirred solution was allowed to warm to room temperature and after standing overnight the dichloromethane solution was washed with a cold saturated aqueous solution of sodium bicarbonate (100 ml). The dichloromethane solution was then dried, treated with charcoal and the solvent removed by distillation under reduced pressure. The residue was washed with diethyl ether to give 5-(p-hydroxyphenoxy)pyrimidine (0.4 g) m.p. 158° C. which was characterised by p.m.r. spectroscopy.

後処理

  1. temperaturethe solution, maintained at a temperature of -70° to -78° C.
  2. washthe dichloromethane solution was washed with a cold saturated aqueous solution of sodium bicarbonate (100 ml)
  3. dry with materialThe dichloromethane solution was then dried
  4. additiontreated with charcoal
  5. customthe solvent removed by distillation under reduced pressure
  6. washThe residue was washed with diethyl ether

出典と根拠

ORDレコード
ord-2ca862c074ec497ea11bc0de5bcc83e4
出典データセット
uspto-grants-1981_02
特許番号
US04248618

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