Sodium borohydride → HCID 17755959, 화합물

HRID 1479252노트

반응식

HRID 1479252 반응식
[OH:1][CH2:2][C:3]1[CH:13]=[CH:12][C:6]([O:7][CH2:8][C:9](=[O:11])[CH3:10])=[CH:5][CH:4]=1.[BH4-].[Na+]>CO.O>[OH:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([O:7][CH2:8][CH:9]([OH:11])[CH3:10])=[CH:12][CH:13]=1

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 177562771-[4-(Hydroxymethyl)phenoxy]propan-2-one

생성물 1

HCID 17755959HCID 17755959, 화합물수율 98%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 1-(4-hydroxymethylphenoxy)-propan-2-one (1.26 g, 6.99 mmol) dissolved in methanol (60 mL) was added solid NaBH4 (0.32 g, 8.39 mmol). After completion of addition the reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with water, and the aqueous layer was extracted with ethyl acetate (3×). All combined organic layers were dried over Na2SO4, filtered, and concentrated to provide an oil (1.24 g, 6.81 mmol), which was used in the next step without any further purification (98% yield). 1H (CDCl37.29, 600 MHz): δ (2H, d, J=8.4 Hz), 6.90 (2H, d, J=8.5 Hz), 4.62 (2H, s), 4.21 (1H, m), 3.94 (1H, dd, J=9.2, 3.1 Hz), 3.82 (1H, m), 1.29 (3H, d, J=6.4 Hz).

후처리

  1. additionAfter completion of addition the reaction mixture
  2. extractionthe aqueous layer was extracted with ethyl acetate (3×)
  3. dry with materialAll combined organic layers were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5a300ceadea9490db13141f310209f90
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09408927B2

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