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2,5,8,11,14,17,20-Heptaoxadocosan-22-amine → HCID 178496251、化合物

HRID 1527633
ノート
印刷プレビュー

反応式

HRID 1527633 の反応式
[N:1]1([C:6]([NH:8][C:9]2[NH:10][C:11]([CH3:16])=[CH:12][C:13](=[O:15])[N:14]=2)=[O:7])[CH:5]=[CH:4]N=C1.C[O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH2:34][CH2:35][O:36][CH2:37]CN>C(OCC)(=O)C>[CH3:37][O:36][CH2:35][CH2:34][O:33][CH2:32][CH2:31][O:30][CH2:29][CH2:28][O:27][CH2:26][CH2:25][O:24][CH2:23][CH2:22][O:21][CH2:20][CH2:19][O:18][CH2:4][CH2:5][NH:1][C:6]([NH:8][C:9]1[NH:10][C:11]([CH3:16])=[CH:12][C:13](=[O:15])[N:14]=1)=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 187646512,5,8,11,14,17,20-Heptaoxadocosan-22-amineHCID 178429402HCID 178429402、化合物

生成物 1

HCID 178496251HCID 178496251、化合物収率 60.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of 4.38 g of 2-(1-imidazolylcarbonylamino)-6-methyl-4[1H]-pyrimidinone 1A (0.02 mol) in 200 ml of ethyl acetate were added 7.4 g of 2,5,8,11,14,17,20 heptaoxadocosan-22-amine (0.0218 mol). The reaction mixture was refluxed for 12 hours. The mixture was then allowed to return to room temperature, and was evaporated under reduced pressure. The residue was taken up in acetone (50 ml) and then filtered to remove the imidazole. The filtrate was evaporated under reduced pressure and then taken up again in 50 ml of acetone and filtered. The filtrate was evaporated under reduced pressure. 5.9 g of the expected product were thus obtained in the form of a pasty oil, in a yield of 60%. 1H and 13C NMR spectra compliant.

後処理

  1. temperatureThe reaction mixture was refluxed for 12 hours
  2. customto return to room temperature
  3. customwas evaporated under reduced pressure
  4. filtrationfiltered
  5. customto remove the imidazole
  6. customThe filtrate was evaporated under reduced pressure
  7. filtrationfiltered
  8. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-c0c3b82db4ff4723bc9c7ea117dc9942
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09089500B2

反応ノート

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