Potassium Carbonate → HCID 10820667, 화합물

HRID 918398노트

반응식

HRID 918398 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][C:9]#[N:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(=O)([O-])[O-].[K+].[K+]>CCOCC.O1CCCC1>[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][NH2:10]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 544562(Tetrahydro-pyran-2-yloxy)-acetonitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 10820667HCID 10820667, 화합물수율 93.3%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 35 g of tetrahydropyran-2-yloxy acetonitrile in 100 ml of ether is added dropwise to a slurry of 10 g of lithium aluminum hydride in 300 ml of ether and 100 ml of tetrahydrofuran. The slurry is refluxed for 210 minutes, cooled, and 25 ml of saturated potassium carbonate solution is added at a rate that maintains gentle reflux. After 90 minutes the slurry is filtered and the solid is washed with ether. The filtrate is evaporated in vacuo and distilled to give 33.6 g of 2-(tetrahydropyran-2-yloxy)-ethylamine, boiling point 41.5° - 46°C at 0.5-0.8 mm.

후처리

  1. temperatureThe slurry is refluxed for 210 minutes
  2. temperaturecooled
  3. filtrationAfter 90 minutes the slurry is filtered
  4. washthe solid is washed with ether
  5. customThe filtrate is evaporated in vacuo
  6. distillationdistilled

출처 및 근거

ORD 기록
ord-73d3ade46bdb4025b974c272003c3cfc
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03971773

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