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Potassium Hydroxide → HCID 12080904, 화합물

HRID 1826063
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HRID 1826063 반응식
[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]
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참가 물질

4

반응물 2

HCID 14797Potassium Hydroxide2회HCID 120809034-(3,5-Bis(methoxycarbonyl)phenyl)-2-methyl-3-butyn-1-ol2회

생성물 1

HCID 12080904HCID 12080904, 화합물수율 97%

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4294a9c50f34262b5839d68d830ed85
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07049371B2

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