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Potassium Hydroxide → HCID 12080904、化合物

HRID 1059053
ノート
印刷プレビュー

反応式

HRID 1059053 の反応式
[OH-].[K+:2].C[O:4][C:5]([C:7]1[CH:8]=[C:9]([C:17]#[C:18]C(C)CO)[CH:10]=[C:11]([C:13]([O:15]C)=[O:14])[CH:12]=1)=[O:6]>C(O)CCC>[C:17]([C:9]1[CH:10]=[C:11]([C:13]([O-:15])=[O:14])[CH:12]=[C:7]([CH:8]=1)[C:5]([O-:6])=[O:4])#[CH:18].[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 Hydroxide2 回HCID 120809034-(3,5-Bis(methoxycarbonyl)phenyl)-2-methyl-3-butyn-1-ol2 回

生成物 1

HCID 12080904HCID 12080904、化合物収率 97%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒2 回

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 182 g (2.763 mole) of potassium hydroxide (85%) were placed and potassium hydroxide was dissolved into n-butanol by heating under the refluxing condition. To the resultant solution, 95 g (0.344 mole) of 4-[3,5-bis(methoxycarbonyl)-phenyl]-2-methyl-3-butyn-1-ol synthesized above in (2) was added and the resultant mixture was heated under the refluxing condition for 30 minutes. The mixture was then cooled in an ice bath. The formed crystals were separated by filtration, washed twice with 1 liter of methanol and dried at 60° C. in vacuo and 88.87 g (the yield: 97%) of dipotassium 5-ethynylisophthalate was obtained.

後処理

  1. customInto a 5 liter four-necked flask equipped with a thermometer
  2. temperatureby heating under the refluxing condition
  3. additionwas added
  4. temperatureThe mixture was then cooled in an ice bath
  5. customThe formed crystals were separated by filtration
  6. washwashed twice with 1 liter of methanol
  7. dry with materialdried at 60° C. in vacuo and 88.87 g (the yield: 97%) of dipotassium 5-ethynylisophthalate
  8. customwas obtained

出典と根拠

ORDレコード
ord-1b9e4e9df6f84b0a9b068c3715214fc1
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06518390B2

反応ノート

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