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Sodium sulfate decahydrate → HCID 2726773, 화합물

HRID 1257463
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HRID 1257463 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 10424923Ethyl 4-[3-(trifluoromethyl)phenyl]-1,3-thiazole-2-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 2726773HCID 2726773, 화합물수율 25%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-11567c222f49457482b0d3a918cf7e3f
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461348B2

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