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Sodium borohydride → 2-(5-Chloro-1,3-dihydro-2-benzofuran-1-yl)ethanol

HRID 2056746
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HRID 2056746 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[CH:6]([CH2:9][C:10](OCC)=[O:11])[O:7][CH2:8][C:4]=2[CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.[BH4-].[Na+]>C1COCC1>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[CH:6]([CH2:9][CH2:10][OH:11])[O:7][CH2:8][C:4]=2[CH:3]=1
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참가 물질

5

반응물 3

HCID 4311764Sodium borohydrideHCID 21225700DiisobutylaluminumhydrideHCID 86592978Ethyl (5-chloro-1,3-dihydro-2-benzofuran-1-yl)acetate

생성물 1

HCID 693065152-(5-Chloro-1,3-dihydro-2-benzofuran-1-yl)ethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl (5-chloro-1,3-dihydro-2-benzofuran-1-yl)-acetate (2.79 g, 11.6 mmol) in THF (60 mL) was cooled to −78° C. and di-isobutylaluminium hydride (1M in toluene) (12.7 mL, 12.7 mmol) was added dropwise. After 1 h, the reaction mixture was quenched with a saturated solution of sodium tartrate (150 mL), allowed to warm to room temperature and stirred for 1 h. The layers were separated and the aqueous layer extracted with ethyl acetate. The combined organic layers were dried (MgSO4), filtered and evaporated in vacuo. The resultant crude intermediate was dissolved in methanol (50 mL), cooled to 0° C., and sodium borohydride (0.48 g, 12.7 mmol) added in portions. The reaction was quenched with saturated sodium hydrogen carbonate and extracted with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and evaporated in vacuo. The crude product was purified by column chromatography, eluting with ethyl acetate/hexane (1:2), to yield the title compound as a white solid.

후처리

  1. customthe reaction mixture was quenched with a saturated solution of sodium tartrate (150 mL)
  2. customThe layers were separated
  3. extractionthe aqueous layer extracted with ethyl acetate
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. dissolutionThe resultant crude intermediate was dissolved in methanol (50 mL)
  8. temperaturecooled to 0° C.
  9. customThe reaction was quenched with saturated sodium hydrogen carbonate
  10. extractionextracted with ethyl acetate
  11. washThe combined organic layers were washed with brine
  12. dry with materialdried (MgSO4)
  13. filtrationfiltered
  14. customevaporated in vacuo
  15. customThe crude product was purified by column chromatography
  16. washeluting with ethyl acetate/hexane (1:2)

출처 및 근거

ORD 기록
ord-0bbe3e3bf7b848448115fcdc0ad9dab6
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07335660B2

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