Potassium Carbonate → HCID 10820667、化合物

HRID 918398ノート

反応式

HRID 918398 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 10820667HCID 10820667、化合物収率 93.3%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-73d3ade46bdb4025b974c272003c3cfc
出典データセット
uspto-grants-1976_07
特許番号
US03971773

反応ノート

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