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Potassium Hydroxide → Dipotassium 5-(2-phenylethynyl)isophthalate

HRID 498158
ノート
印刷プレビュー

反応式

HRID 498158 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]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:10]=[C:11]([C:13]([O:15]C)=[O:14])[CH:12]=1)=[O:6]>C(O)CCC>[C:19]1([C:18]#[C:17][C:9]2[CH:10]=[C:11]([C:13]([O-:15])=[O:14])[CH:12]=[C:7]([CH:8]=2)[C:5]([O-:6])=[O:4])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[K+:2].[K+:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 10946313dimethyl 5-phenylethynylisophthalate

生成物 1

HCID 12080907Dipotassium 5-(2-phenylethynyl)isophthalate収率 97%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

Into a 5 liter four-necked flask equipped with a thermometer, a Dimroth condenser and a stirrer, 3 liters of n-butanol and 180 g (2.72 moles) of potassium hydroxide (85%) were placed and dissolved by heating under the refluxing condition. To the obtained solution, 80 g (0.272 moles) of (3,5-bis(methoxycarbonyl)phenyl)-2-phenylethyne synthesized above was added and the resultant mixture was heated for 30 minutes under the refluxing condition. The reaction mixture was then cooled in an ice bath and the formed crystals were separated by filtration. The crystals were washed twice with 1 liter of ethanol and dried at 60° C. under a reduced pressure and 90.35 g of dipotassium 5-(2-phenylethynyl)-isophthalate was obtained (the yield: 97%).

後処理

  1. customInto a 5 liter four-necked flask equipped with a thermometer
  2. dissolutiondissolved
  3. temperatureby heating under the refluxing condition
  4. additionabove was added
  5. temperatureThe reaction mixture was then cooled in an ice bath
  6. customthe formed crystals were separated by filtration
  7. washThe crystals were washed twice with 1 liter of ethanol
  8. customdried at 60° C. under a reduced pressure

出典と根拠

ORDレコード
ord-c447c8e6758a4491975f397b5169b8e7
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949674B2

反応ノート

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