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Sodium borohydride → HCID 66778553, 화합물

HRID 2091377
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HRID 2091377 반응식
[F:1][C:2]1[C:7]2[C:8]([CH3:16])=[C:9]([C:11](=[O:15])[CH:12]([CH3:14])[CH3:13])[O:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+]>O1CCCC1.CO>[F:1][C:2]1[C:7]2[C:8]([CH3:16])=[C:9]([CH:11]([OH:15])[CH:12]([CH3:13])[CH3:14])[O:10][C:6]=2[CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 66778352HCID 66778352, 화합물2회

생성물 1

HCID 66778553HCID 66778553, 화합물수율 99.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

1-(4-Fluoro-3-methyl-1-benzofuran-2-yl)-2-methylpropan-1-one (1.4 g) synthesized in the above-mentioned (1) was dissolved in tetrahydrofuran (20 mL) and methanol (2 mL), and sodium borohydride (90%, 0.53 g) was added to the solution under ice-cooling. The ice bath was removed, and the reaction mixture was stirred at room temperature for 1 hr then ice-cooled again, and water (2 mL) and 1N hydrochloric acid (5 mL) were carefully added to the mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure to give a crude product (1.4 g, quantitative) of the title object compound as a pale-yellow oil.

후처리

  1. temperaturecooling
  2. customThe ice bath was removed
  3. temperatureice-cooled again
  4. additionwater (2 mL) and 1N hydrochloric acid (5 mL) were carefully added to the mixture
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e97cbc9e194d4f93bb155150e6a685ba
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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