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

HRID 431585ノート

反応式

HRID 431585 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-e305bc908ba848eea2fa7046266b0bba
出典データセット
uspto-grants-2003_12
特許番号
US06660736B2

反応ノート

読み込み中…