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Methanol → HCID 20079668, 화합물

HRID 2203004
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HRID 2203004 반응식
[F:1][CH:2]([F:12])[C:3]1[S:7][C:6]([C:8](OC)=[O:9])=[CH:5][CH:4]=1.CO.[BH4-].[Na+]>C1COCC1>[F:1][CH:2]([F:12])[C:3]1[S:7][C:6]([CH2:8][OH:9])=[CH:5][CH:4]=1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 54464229Methyl 5-(difluoromethyl)thiophene-2-carboxylate

생성물 1

HCID 20079668HCID 20079668, 화합물수율 101.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a solution of methyl 5-(difluoromethyl)thiophene-2-carboxylate (2.23 g) in THF (60 ml)-MeOH (15 ml) was added NaBH4 (2.20 g) at room temperature, and the reaction mixture was stirred at 60° C. for 1 h. The reaction mixture was quenched with saturated aqueous NH4Cl solution, and extracted with EtOAc. The extract was washed with brine, dried over MgSO4, concentrated and purified by silica gel column chromatography (hexane/EtOAc) to give the title compound (1.94 g) as a pale yellow oil.

후처리

  1. customThe reaction mixture was quenched with saturated aqueous NH4Cl solution
  2. extractionextracted with EtOAc
  3. washThe extract was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. custompurified by silica gel column chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-d63bc354b72d4b229efa01715e85bb3b
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365540B2

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