Water → 2,3-Dihydro-1H-pyrido[2,3-b][1,4]oxazine

HRID 1943626노트

반응식

HRID 1943626 반응식
[NH:1]1[C:6](=O)[CH2:5][O:4][C:3]2[N:8]=[CH:9][CH:10]=[CH:11][C:2]1=2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH:1]1[CH2:6][CH2:5][O:4][C:3]2[N:8]=[CH:9][CH:10]=[CH:11][C:2]1=2

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 159259881H,2H,3H-pyrido(2,3-b)(1,4)oxazin-2-oneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 151279022,3-Dihydro-1H-pyrido[2,3-b][1,4]oxazine수율 88.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

1H-pyrido[2,3-b][1,4]oxazin-2-one (113 mg, 0.75 mmol) was dissolved in tetrahydrofuran (3.5 ml) and then cooled to 0□. 1.0M Lithium aluminum hydride dissolved in tetrahydrofuran (1.5 ml, 1.5 mmol) was added thereto dropwise. After stirring for 2 hours at room temperature, 0.1 ml of water, 0.2 ml of 10% aqueous solution of sodium hydroxide, and 0.3 ml of water were added in this order under stirring. After filtering precipitates, the filtrate was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain colorless liquid (90 mg, 88%).

후처리

  1. temperaturecooled to 0□
  2. additionwas added
  3. stirringunder stirring
  4. filtrationAfter filtering
  5. customprecipitates
  6. extractionthe filtrate was extracted with ethyl acetate
  7. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
  8. filtrationfiltered
  9. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-9b39bdf8a3164714a71fc4810a2a0710
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394792B2

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