4-Methylmorpholine → HCID 22560972, 화합물

HRID 983512노트

반응식

HRID 983512 반응식
[OH:1][CH2:2][CH2:3][CH2:4][NH:5][C:6](=[O:22])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].CN1CCOCC1.Cl[C:31]([O:33][CH2:34][CH3:35])=[O:32]>O1CCCC1>[CH2:34]([O:33][C:31]([O:1][CH2:2][CH2:3][CH2:4][NH:5][C:6](=[O:22])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[O:32])[CH3:35]

참가 물질

5

반응물 3

HCID 79724-MethylmorpholineHCID 10928Ethyl chloroformateHCID 9922829N-(3-hydroxypropyl)hexadecanamide

생성물 1

HCID 22560972HCID 22560972, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3.14 g of N-(3-hydroxypropyl) hexadecanamide (10 mmoles) was suspended in 75 ml of tetrahydrofuran (THF) at 45° C. with stirring. 1.11 g of N-methylmorpholine (11 mmoles) and 1.19 g of ethyl chloroformate (11 mmoles) were added and the resulting mixture was stirred for a further 3 hours at ambient temperature. The mixture was then evaporated to dryness under vacuum. The residue was taken up with 50 ml of water and extracted 3 times with 30 ml of ethyl acetate; the organic phases were washed twice with 20 ml of water, recombined and evaporated to dryness. The residue was crystallized from 30 ml of tert-butylmethyl ether. The crystallizate was separated by filtration, washed twice with 5 ml of cold tert-butylmethyl ether and finally dried in a high degree of vacuum. The yield of the reaction was 92%.

후처리

  1. stirringthe resulting mixture was stirred for a further 3 hours at ambient temperature
  2. customThe mixture was then evaporated to dryness under vacuum
  3. extractionextracted 3 times with 30 ml of ethyl acetate
  4. washthe organic phases were washed twice with 20 ml of water
  5. customevaporated to dryness
  6. customThe residue was crystallized from 30 ml of tert-butylmethyl ether
  7. customThe crystallizate was separated by filtration
  8. washwashed twice with 5 ml of cold tert-butylmethyl ether
  9. customfinally dried in a high degree of vacuum

출처 및 근거

ORD 기록
ord-aebfee80452848fcb97ecf2b9b8582f8
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06864285B1

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