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Sodium sulfate decahydrate → HCID 2726773、化合物

HRID 1257463
ノート
印刷プレビュー

反応式

HRID 1257463 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]([F:26])([F:25])[C:9]1[CH:10]=[C:11]([C:15]2[N:16]=[C:17]([C:20](OCC)=[O:21])[S:18][CH:19]=2)[CH:12]=[CH:13][CH:14]=1.O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[F:26][C:8]([F:7])([F:25])[C:9]1[CH:10]=[C:11]([C:15]2[N:16]=[C:17]([CH2:20][OH:21])[S:18][CH:19]=2)[CH:12]=[CH:13][CH:14]=1
参加物反応条件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 62649Sodium sulfate decahydrateHCID 10424923Ethyl 4-[3-(trifluoromethyl)phenyl]-1,3-thiazole-2-carboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 2726773HCID 2726773、化合物収率 25%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

Under a nitrogen atmosphere at 0° C., to a solution (50 mL) of lithium aluminum hydride (710 mg, 19 mmol) in tetrahydrofuran was added dropwise a solution (40 mL) of the compound (5.6 g, 19 mmol) obtained in Example 190a in tetrahydrofuran, and the mixture was stirred at 0° C. for 3 hr. After confirmation of the termination of the reaction by TLC, sodium sulfate 10 hydrate was added to the reaction mixture, and the mixture was stirred at room temperature overnight. The resulting salt was removed and the solvent was evaporated under reduced pressure. The obtained crude product was purified by column chromatography (hexane-hexane/ethyl acetate=70/30) to give the title compound (1.2 g, 25%) as an orange oil.

後処理

  1. additionwas added to the reaction mixture
  2. stirringthe mixture was stirred at room temperature overnight
  3. customThe resulting salt was removed
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained crude product
  6. customwas purified by column chromatography (hexane-hexane/ethyl acetate=70/30)

出典と根拠

ORDレコード
ord-11567c222f49457482b0d3a918cf7e3f
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

反応ノート

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