Ethyl Acetate → Stearyl-[3-(p-dimethylaminobenzamido) propyl]-Dimethylammonium p-toluenesulfonate

HRID 2399656

反応式

HRID 2399656 の反応式
[CH3:1][N:2]([CH3:18])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([N:14]([CH3:16])[CH3:15])=[CH:10][CH:9]=1.[CH2:19]([O:37][S:38]([C:41]1[CH:46]=[CH:45][C:44]([CH3:47])=[CH:43][CH:42]=1)(=[O:40])=[O:39])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]C.[CH2:48](OC(=O)C)C>>[C:44]1([CH3:47])[CH:43]=[CH:42][C:41]([S:38]([O-:40])(=[O:37])=[O:39])=[CH:46][CH:45]=1.[CH2:18]([N+:2]([CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:17])[C:8]1[CH:9]=[CH:10][C:11]([N:14]([CH3:16])[CH3:15])=[CH:12][CH:13]=1)([CH3:48])[CH3:1])[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH3:19]

参加物

4

反応物 3

HCID 8857Ethyl AcetateHCID 229551Octadecyl p-ToluenesulfonateHCID 39788884-(dimethylamino)-N-[3-(dimethylamino)propyl]benzamide

生成物 1

HCID 19382935Stearyl-[3-(p-dimethylaminobenzamido) propyl]-Dimethylammonium p-toluenesulfonate

実験手順

N-(3-dimethylaminopropyl)-p-dimethylaminobenzamide (77 g, 0.31 mole) from Example 1 and 131.5 g of stearyl-p-toluenesulfonate (0.31 mole) was heated to 110° C. under a blanket of nitrogen with continuous stirring for 2 hours. The resulting melt was dissolved in 800 ml of hot ethylacetate and then crystallized by cooling to ambient temperature. The crystals were recovered by filtration, dried in air and then under vacuum at 50°-60° C. The resulting whitish crystals of stearyl-[3-(p-dimethyl-aminobenzamido)propyl]dimethyl ammonium p-toluenesulfonate were found to have a melting point of 122°-125° C. and the yield 191.8 g, was 92% of theoretical. The structure and purity of the product were confirmed by elemental analysis, NMR, FTIR and UV spectra.

後処理

  1. customcrystallized
  2. filtrationThe crystals were recovered by filtration
  3. customdried in air
  4. customat 50°-60° C

出典と根拠

ORDレコード
ord-a41d129298094c218abea644cb34c047
出典データセット
uspto-grants-1995_09
特許番号
US05451394

関連ノート

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