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Diethyl Ether → HCID 86626342, 화합물

HRID 907606
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HRID 907606 반응식
[F:1][C:2]([F:17])([O:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=1)[C:3]([N:5]([O:7][CH3:8])[CH3:6])=[O:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].C(OCC)C>C1COCC1>[F:17][C:2]([F:1])([O:9][C:10]1[CH:11]=[CH:12][C:13]([F:16])=[CH:14][CH:15]=1)[CH:3]([N:5]([O:7][CH3:8])[CH3:6])[OH:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 86626341HCID 86626341, 화합물

생성물 1

HCID 86626342HCID 86626342, 화합물수율 57%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 2,2-difluoro-2-(4-fluorophenoxy)-N-methoxy-N-methylacetamide (2.03 g, 8.1 mmol) in anhydrous THF (15 ml) at 0° C., a solution of 1 M of lithium aluminum hydride in THF (4.05 ml, 4.05 mmol) was added. After stirring the solution for 3 h, 1N NaOH (2 ml) and ethyl ether (15 ml) were added. After 30 min, the reaction mixture was filtered through Celite and the cake was washed several times with ethyl ether. The organic phase was washed with brine and dried over sodium sulfate. The solvent was removed and the crude was purified using a short plug of silica gel to give 2,2-difluoro-2-(4-fluorophenoxy)-1-(N-methoxy-N-methylamino)ethanol as an oil (1.15 g, 57%).

후처리

  1. waitAfter 30 min
  2. filtrationthe reaction mixture was filtered through Celite
  3. washthe cake was washed several times with ethyl ether
  4. washThe organic phase was washed with brine
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed
  7. customthe crude was purified

출처 및 근거

ORD 기록
ord-f4c717a4e68542428b63f88100eca090
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08013186B2

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