Water → 2-Allyloxymethyl-4-n-propylmorpholine

HRID 1283005노트

반응식

HRID 1283005 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydride2회HCID 538376442-Allyloxymethyl-4-n-propylmorpholin-5-one

생성물 1

HCID 214304122-Allyloxymethyl-4-n-propylmorpholine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b052377bae52464ea1783f0315e81381
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03974156

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