3,4-dihydro-2H-pyran → 1-(4'-(2-Tetrahydropyranyloxy)phenyl)-3-bromopropane

HRID 2227106ノート

反応式

HRID 2227106 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][Br:11])=[CH:4][CH:3]=1.[O:12]1[CH:17]=[CH:16][CH2:15][CH2:14][CH2:13]1.C(=O)([O-])[O-].[K+].[K+]>ClCCl.P(Cl)(Cl)(Cl)=O>[O:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]1[O:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][Br:11])=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 80803,4-dihydro-2H-pyranHCID 11430Potassium CarbonateHCID 148170364-(3-Bromopropyl)phenol

生成物 1

HCID 184717901-(4'-(2-Tetrahydropyranyloxy)phenyl)-3-bromopropane

試薬・触媒・溶媒 2

HCID 24813Phosphorus oxychloride触媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 1-(4′-hydroxyphenyl)-3-bromopropane 3B (3.56 g) in dichloromethane (11 mL) is added dihydropyran (2.3 mL). The reaction mixture is cooled to 0° C., and three drops of phosphorus oxychloride are added. The reaction mixture is stirred in the ice bath for a further two hours, then gradually allowed to warm to room temperature, where it is allowed to stir overnight. To the reaction mixture is then added potassium carbonate (3 g), and the reaction mixture is stirred an additional hour. The solid is then filtered out, and the solvents and residual DHP is removed in vacuo.

後処理

  1. temperatureto warm to room temperature
  2. filtrationThe solid is then filtered out
  3. customthe solvents and residual DHP is removed in vacuo

出典と根拠

ORDレコード
ord-3936bb0374a549fba4004c4ecbb16f12
出典データセット
uspto-grants-2002_07
特許番号
US06413448B1

反応ノート

読み込み中…