Potassium Hydroxide → 5-(1-Adamantylethynyl)isophthalic acid dipotassium salt

HRID 1994660ノート

反応式

HRID 1994660 の反応式
[OH-].[K+:2].C[O:4][C:5]([C:7]1[CH:8]=[C:9]([C:17]#[C:18][C:19]23[CH2:28][CH:23]4[CH2:24][CH:25]([CH2:27][CH:21]([CH2:22]4)[CH2:20]2)[CH2:26]3)[CH:10]=[C:11]([C:13]([O:15]C)=[O:14])[CH:12]=1)=[O:6]>C(O)CCC>[K+:2].[K+:2].[C:19]12([C:18]#[C:17][C:9]3[CH:10]=[C:11]([C:13]([O-:15])=[O:14])[CH:12]=[C:7]([CH:8]=3)[C:5]([O-:6])=[O:4])[CH2:20][CH:21]3[CH2:22][CH:23]([CH2:24][CH:25]([CH2:27]3)[CH2:26]1)[CH2:28]2

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 675073001-(3,5-Bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne

生成物 1

HCID 675066175-(1-Adamantylethynyl)isophthalic acid dipotassium salt収率 97%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

In a 5 L four-neck flask provided with a thermometer, a Dimroth condenser and an agitator, 3 L of n-butanol and 226 g of potassium hydroxide (85%) (2.72 mol) were charged. The mixture was heated and refluxed to be dissolved. After adding 120 g of the obtained 1-(3,5-bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne (0.341 mol) therein, the mixture was heated and refluxed for 30 minutes. Next, it was cooled in an ice bath and filtered to obtain precipitated crystal. The crystal was washed with 1 L of ethanol two times followed by drying under pressure at 60° C., thus obtaining 132.49 g of 5-(2-(1-adamantyl)ethynyl) isophthalic acid dipotassium salt (the yield was 97%).

後処理

  1. customIn a 5 L four-neck flask provided with a thermometer
  2. temperatureThe mixture was heated
  3. temperaturerefluxed
  4. dissolutionto be dissolved
  5. temperaturethe mixture was heated
  6. temperaturerefluxed for 30 minutes
  7. temperatureNext, it was cooled in an ice bath
  8. filtrationfiltered
  9. customto obtain
  10. customprecipitated crystal
  11. washThe crystal was washed with 1 L of ethanol two times
  12. customby drying under pressure at 60° C.

出典と根拠

ORDレコード
ord-13a4d2f0e7544239ab7abc05a4ff91b6
出典データセット
uspto-grants-2010_01
特許番号
US07652125B2

反応ノート

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