Water → HCID 23614758、化合物

HRID 1768131ノート

反応式

HRID 1768131 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:12][CH2:11][CH2:10][C:9]2=[O:13])=[CH:4][CH:3]=1.[F:14][C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH2:18]Br.C(=O)([O-])[O-].[K+].[K+].O>CC(=O)CC.C(OCC)(=O)C>[F:14][C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH2:18][O:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:12][CH2:11][CH2:10][C:9]2=[O:13])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 680073-Fluorobenzyl bromideHCID 7855861-(4-hydroxyphenyl)pyrrolidin-2-one

生成物 1

HCID 23614758HCID 23614758、化合物収率 88%

試薬・触媒・溶媒 2

HCID 6569Methyl Ethyl Ketone溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2.73 g (15.4 mmol) of 1-(4-hydroxy-phenyl)-pyrrolidin-2-one, 3.2 g (16.9 mmol) of 3-fluorobenzylbromide and 4.26 g (31 mmol) of potassium carbonate in 100 ml of 2-butanone is heated at 80° C. for 18 hours. After cooling to RT, the reaction mixture is treated with water and ethyl acetate. The organic layer is separated, dried over magnesium sulfate and evaporated under reduced pressure. The solid residue is crystallised from ether to yield 3.86 g (88% of theory) of 1-[4-(3-fluoro-benzyloxy)-phenyl]-pyrrolidin-2-one as a colorless solid. MS: m/e=286.0 (M+H)+.

後処理

  1. temperatureAfter cooling to RT
  2. customThe organic layer is separated
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure
  5. customThe solid residue is crystallised from ether

出典と根拠

ORDレコード
ord-bfaab34fd87d4736bf247b26c428ce39
出典データセット
uspto-grants-2007_06
特許番号
US07235581B2

反応ノート

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