Sodium Carbonate → HCID 22750168, Verbindung

HRID 1283973

Reaktionsgleichung

Reaktionsgleichung von HRID 1283973
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][C:18]=1[O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:12](=[O:15])[CH2:13]Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:27]([CH2:30][C:31]1[CH:47]=[CH:46][C:34]([O:35][CH2:36][CH2:37][NH:38][CH2:39][C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)=[CH:33][CH:32]=1)(=[O:29])[NH2:28].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH2:39]([N:38]([CH2:37][CH2:36][O:35][C:34]1[CH:33]=[CH:32][C:31]([CH2:30][C:27](=[O:29])[NH2:28])=[CH:47][CH:46]=1)[CH2:13][C:12](=[O:15])[C:11]1[CH:16]=[CH:17][C:18]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:10]=1)[C:40]1[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=1

Komponenten

5

Versuchsvorschrift

A mixture 3,4-dibenzyloxyphenacyl bromide (32.8 g.), N-[2-(4-carbamoylmethylphenoxy)ethyl]benzylamine (22.8 g.), anhydrous sodium carbonate (8.4 g.) and ethanol (1 liter) was boiled under reflux for 3 hours, then filtered hot to remove the inorganic sediment and evaporated in vacuo to afford a thick syrup. The latter was recrystallized upon trituration in diethyl ether and a sample of the resultant solid was recrystallized from ethanol to give N-benzyl-N-(3,4-dibenzyloxybenzoyl)methyl-2-(4-carbamoylmethylphenoxy)ethylamine, m.p. 99°- 101°C.

Aufarbeitung

  1. temperatureunder reflux for 3 hours
  2. filtrationfiltered hot
  3. customto remove the inorganic sediment
  4. customevaporated in vacuo
  5. customto afford a thick syrup
  6. customThe latter was recrystallized upon trituration in diethyl ether
  7. customa sample of the resultant solid was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-52da37c7eb46456baa9fc70aae950032
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03976783

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