Benzene → 2-[2-[2-[4-(Diphenylmethylene)-1-piperidinyl]ethoxy]ethoxy]-acetamide

HRID 325889Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 325889
[C:1]1([C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:21][CH2:22][O:23][CH2:24][CH2:25][O:26][CH2:27][C:28]([NH2:30])=[O:29].C(=O)([O-])[O-].[Na+].[Na+].C1C=CC=CC=1>C1(C)C(C)=CC=CC=1>[C:1]1([C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[C:8]2[CH2:9][CH2:10][N:11]([CH2:21][CH2:22][O:23][CH2:24][CH2:25][O:26][CH2:27][C:28]([NH2:30])=[O:29])[CH2:12][CH2:13]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

6

Edukt 4

HCID 241BenzeneHCID 10340Sodium CarbonateHCID 27625334-(Diphenylmethylene)piperidineHCID 204631532-[2-(2-Chloroethoxy)ethoxy]-acetamide

Produkt 1

HCID 204631512-[2-[2-[4-(Diphenylmethylene)-1-piperidinyl]ethoxy]ethoxy]-acetamideAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A mixture of 29.9 g of 4-(diphenylmethylene)-piperidine, 36.3 g of 2-[2-(2-chloroethoxy)ethoxy]-acetamide and 18 g of sodium carbonate in 80 ml of xylene is heated for 20 hours at a temperature of from 90°to 110° C. Thereafter, 80 ml of benzene are added thereto. The precipitate obtained is filtered off and the organic phase is extracted with a dilute solution of hydrochloric acid (20 ml of concentrated hydrochloride acid and 80 ml of water). After the addition of 30 ml of a concentrated solution of sodium hydroxide and extraction with benzene, the benzene solution obtained is washed, dried over anhydrous potassium carbonate and the benzene evaporated in vacuo. The 2-[2-[2-[4-(diphenylmethylene)-1-piperidinyl]ethoxy]ethoxy]-acetamide obtained is used as such for the preparation of the corresponding acid (see Example 3.4).

Aufarbeitung

  1. customThe precipitate obtained
  2. filtrationis filtered off
  3. extractionthe organic phase is extracted with a dilute solution of hydrochloric acid (20 ml of concentrated hydrochloride acid and 80 ml of water)
  4. additionAfter the addition of 30 ml of a concentrated solution of sodium hydroxide and extraction with benzene
  5. customthe benzene solution obtained
  6. washis washed
  7. dry with materialdried over anhydrous potassium carbonate
  8. customthe benzene evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-55c13fe774414739968eaee76683f1c2
Quelldatensatz
uspto-grants-1984_04
Patentnummer
US04443460

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