Potassium Carbonate → 5-(4-Fluoro-benzyloxy)-2-(2-methoxy-ethyl)-isoindole-1,3-dione

HRID 1070687노트

반응식

HRID 1070687 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[N:6]([CH2:12][CH2:13][O:14][CH3:15])[C:5]2=[O:16].C(=O)([O-])[O-].[K+].[K+].[F:23][C:24]1[CH:31]=[CH:30][C:27]([CH2:28]Br)=[CH:26][CH:25]=1>CC(C)=O>[F:23][C:24]1[CH:31]=[CH:30][C:27]([CH2:28][O:1][C:2]2[CH:3]=[C:4]3[C:8](=[CH:9][CH:10]=2)[C:7](=[O:11])[N:6]([CH2:12][CH2:13][O:14][CH3:15])[C:5]3=[O:16])=[CH:26][CH:25]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 680214-Fluorobenzyl bromideHCID 148489615-Hydroxy-2-(2-methoxy-ethyl)-isoindole-1,3-dione

생성물 1

HCID 102367635-(4-Fluoro-benzyloxy)-2-(2-methoxy-ethyl)-isoindole-1,3-dione수율 66%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 5-hydroxy-2-(2-methoxy-ethyl)-isoindole-1,3-dione, from example 13a, (570 mg, 2.6 mmol), potassium carbonate (445 mg, 3.2 mmol) and 4-fluorobenzyl-bromide (526 mg, 2.8 mmol) in acetone (40 mL) was heated under reflux for 17 h. After cooling to room temperature, the mixture was filtered, evaporated and the residue was purified by crystallization from diethylether:heptane (1:2) to afford the title compound (560 mg, 66%) as a white solid. MS: m/e=330.4 (M+H+).

후처리

  1. temperatureunder reflux for 17 h
  2. filtrationthe mixture was filtered
  3. customevaporated
  4. customthe residue was purified by crystallization from diethylether:heptane (1:2)

출처 및 근거

ORD 기록
ord-94e15c6b9bab40108d7c52beff9e4afd
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903095B2

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