Sodium sulfate decahydrate → HCID 68663620, 화합물

HRID 452636노트

반응식

HRID 452636 반응식
[CH3:1][S:2][C:3]1[CH:12]=[CH:11][C:6]([C:7](OC)=[O:8])=[CH:5][C:4]=1[C:13]([F:16])([F:15])[F:14].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][S:2][C:3]1[CH:12]=[CH:11][C:6]([CH2:7][OH:8])=[CH:5][C:4]=1[C:13]([F:14])([F:15])[F:16]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 68664439HCID 68664439, 화합물

생성물 1

HCID 68663620HCID 68663620, 화합물수율 95.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 4-(methylthio)-3-(trifluoromethyl)benzoate (10.0 g, 40.0 mmol) in tetrahydrofuran (100 mL) was added lithium aluminum hydride (1.52 g, 40.0 mmol) at 0° C. by small portions, and the resulting mixture was stirred for 15 min. Sodium sulfate decahydrate (12.9 g, 40.0 mmol) was added to the reaction mixture by small portions, and the obtained mixture was further stirred at room temperature for 1 hr. Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1), and crystallized from hexane/ethyl acetate to give the title compound (8.46 g, yield 95%) as colorless crystals.

후처리

  1. stirringthe obtained mixture was further stirred at room temperature for 1 hr
  2. filtrationInsoluble material was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1)
  5. customcrystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-1bb689f3aac04b25a15a787a1b9b6a07
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492378B2

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