Water → 2-(4-Chloro-2-butenyl)-1,3-isoindolinedione

HRID 1642097

反応式

HRID 1642097 の反応式
[Cl:1][CH2:2]/[CH:3]=[CH:4]/[CH2:5]Cl.[C:7]([NH2:18])(=[O:17])[C:8]1[C:9](=[CH:13][CH:14]=[CH:15][CH:16]=1)[C:10](N)=[O:11].[K].O>CN(C=O)C>[Cl:1][CH2:2][CH:3]=[CH:4][CH2:5][N:18]1[C:7](=[O:17])[C:8]2[C:9](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:10]1=[O:11]

参加物

5

反応物 3

HCID 962WaterHCID 6421971,4-Dichloro-2-butene, (2E)-HCID 53445390Potassium phthalamide

生成物 1

HCID 27342002-(4-Chloro-2-butenyl)-1,3-isoindolinedione収率 76%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Trans-1,4-dichloro-2-butene (1.14 ml, 10.8 mmol) was dissolved in DMF (27 ml) and purged with argon. Potassium pthalamide (1.00 g, 5.40 mmol) was added to the solution and the reaction was allowed to stir at room temperature overnight. The reaction was then poured into water (75 ml), which precipitated a white solid. This solid was collected by filtration and purified using silica gel chromatography (3:1 Hex:EtOAc) to afford a 76% yield (961 mg) of a white solid.

後処理

  1. custompurged with argon
  2. customprecipitated a white solid
  3. filtrationThis solid was collected by filtration
  4. custompurified

出典と根拠

ORDレコード
ord-f81910309c004b8eace99061811cd35d
出典データセット
uspto-grants-2012_02
特許番号
US08119642B2

関連ノート

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