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Citric Acid → HCID 45121755, 화합물

HRID 2246163
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HRID 2246163 반응식
C(=O)([O-])[O-].[K+].[K+].C[Si](C)(C)[C:9]#[C:10][C:11]1[S:15][CH:14]=[N:13][C:12]=1[CH2:16][OH:17].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CO>[C:10]([C:11]1[S:15][CH:14]=[N:13][C:12]=1[CH2:16][OH:17])#[CH:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 311Citric AcidHCID 11430Potassium CarbonateHCID 592179795-[2-(Trimethylsilyl)ethynyl]-4-thiazolemethanol

생성물 1

HCID 45121755HCID 45121755, 화합물수율 78.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Potassium carbonate (39 mg) was added to a solution of 6.02 g of [5-[2-(trimethylsilyl)ethynyl]thiazol-4-yl]-methanol in 12 ml of methanol, and the mixture was stirred at room temperature for 10 min. A 10% aqueous citric acid solution (6 ml) was added thereto, and the mixture was stirred for 30 min. The reaction mixture was then extracted with 90 ml of ethyl acetate. The organic layer was washed with 12 ml of 5% sodium bicarbonate water and 12 ml of 20% brine in that order and was treated with 0.8 g of activated carbon and anhydrous magnesium sulfate. Toluene (15 ml) was added to the organic layer, the mixture was concentrated, and the precipitated solid was collected by filtration to give 3.11 g of 5-ethynyl-4-hydroxymethylthiazole.

후처리

  1. stirringthe mixture was stirred for 30 min
  2. extractionThe reaction mixture was then extracted with 90 ml of ethyl acetate
  3. washThe organic layer was washed with 12 ml of 5% sodium bicarbonate water and 12 ml of 20% brine in that order
  4. additionwas treated with 0.8 g of activated carbon and anhydrous magnesium sulfate
  5. additionToluene (15 ml) was added to the organic layer
  6. concentrationthe mixture was concentrated
  7. filtrationthe precipitated solid was collected by filtration

출처 및 근거

ORD 기록
ord-2f0a1f29bb5049a298e4ab72e12a6333
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07687490B2

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