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Citric Acid → HCID 45121755、化合物

HRID 2246163
ノート
印刷プレビュー

反応式

HRID 2246163 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 45121755HCID 45121755、化合物収率 78.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2f0a1f29bb5049a298e4ab72e12a6333
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07687490B2

反応ノート

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