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

HRID 1070687ノート

反応式

HRID 1070687 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-94e15c6b9bab40108d7c52beff9e4afd
出典データセット
uspto-grants-2005_06
特許番号
US06903095B2

反応ノート

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