4-Methylmorpholine → HCID 22560972、化合物

HRID 983512ノート

反応式

HRID 983512 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 22560972HCID 22560972、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-aebfee80452848fcb97ecf2b9b8582f8
出典データセット
uspto-grants-2005_03
特許番号
US06864285B1

反応ノート

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