Sodium borohydride → HCID 59255152, 화합물

HRID 78229

반응식

HRID 78229 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][C:7]=1[F:14].[BH4-].[Na+]>CO>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:13]=[CH:12][C:9]([CH2:10][OH:11])=[CH:8][C:7]=1[F:14]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 592554594-[1,3]Dioxolan-2-yl-3-fluoro-benzaldehyde

생성물 1

HCID 59255152HCID 59255152, 화합물수율 24.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a methanol solution (200 mL) of 4-[1,3]dioxolan-2-yl-3-fluoro-benzaldehyde (10 g, 50.9 mmol) described in Manufacturing Example 204-1-2 was added sodium borohydride (2.12 g, 56 mmol), which was stirred for 1 hour at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (2.44 g, 24%).

후처리

  1. customThis mixture was partitioned into ethyl acetate and water
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under a reduced pressure
  7. customthe residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1)

출처 및 근거

ORD 기록
ord-5127a859fdf9415abc4f22d116eaadaf
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841327B2

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