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

HRID 2227106노트

반응식

HRID 2227106 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 24813Phosphorus oxychloride촉매HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3936bb0374a549fba4004c4ecbb16f12
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06413448B1

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