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Ammonium Chloride → HCID 20079668, 화합물

HRID 1497374
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HRID 1497374 반응식
[F:1][CH:2]([F:12])[C:3]1[S:7][C:6]([C:8](OC)=[O:9])=[CH:5][CH:4]=1.[BH4-].[Na+].[Cl-].[NH4+]>O1CCCC1.CO>[F:1][CH:2]([F:12])[C:3]1[S:7][C:6]([CH2:8][OH:9])=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 54464229Methyl 5-(difluoromethyl)thiophene-2-carboxylate

생성물 1

HCID 20079668HCID 20079668, 화합물수율 101.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매
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온도
60 °C

실험 절차

To a mixed solution of methyl 5-(difluoromethyl)thiophene-2-carboxylate (2.23 g) in tetrahydrofuran (60 ml) and methanol (15 ml) was added sodium borohydride (2.2 g) at room temperature, and the mixture was stirred at 60° C. for 1 hr. The reaction mixture was cooled to room temperature, saturated aqueous ammonium chloride solution was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.94 g).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-55ea9f3c517041628620183d3a26ebe3
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09199963B2

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