Water → 2-Allyloxymethyl-4-n-propylmorpholine

HRID 1283104ノート

反応式

HRID 1283104 の反応式
[CH2:1]([O:4][CH2:5][CH:6]1[O:11][CH2:10][C:9](=O)[N:8]([CH2:13][CH2:14][CH3:15])[CH2:7]1)[CH:2]=[CH2:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].O>CCOCC>[CH2:1]([O:4][CH2:5][CH:6]1[O:11][CH2:10][CH2:9][N:8]([CH2:13][CH2:14][CH3:15])[CH2:7]1)[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydride2 回HCID 538376442-Allyloxymethyl-4-n-propylmorpholin-5-one

生成物 1

HCID 214304122-Allyloxymethyl-4-n-propylmorpholine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 2-allyloxymethyl-4-n-propylmorpholin-5-one (65 g.) in dry ether (100 ml.) is added slowly with stirring to a suspension of lithium aluminium hydride (17.5 g.) in dry ether (700 ml.). The rate of addition is adjusted so that the reaction mixture refluxes gently. When the addition is complete the reaction mixture is stirred at ambient temperature (18°-20°C.) for 18 hours and then water (90 ml.) is added very carefully dropwise to decompose the complex and excess of lithium aluminium hydride. The ethereal solution is filtered and the solid residue is washed with ether. The filtrate and ethereal washings are combined, dried (Na2SO4), filtered and the ether evaporated. The product, 2-allyloxymethyl-4-n-propylmorpholine is obtained as an oil b.p. 80°-90°C. at 1 m.m. which forms a hydrogen oxalate, m.p. 125°-127°C.

後処理

  1. additionThe rate of addition
  2. additionWhen the addition
  3. filtrationThe ethereal solution is filtered
  4. washthe solid residue is washed with ether
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customthe ether evaporated

出典と根拠

ORDレコード
ord-cab892ce522440ce81f4daa844e984aa
出典データセット
uspto-grants-1976_08
特許番号
US03974158

反応ノート

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