Pyridine → Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate

HRID 414242

Reaktionsgleichung

Reaktionsgleichung von HRID 414242
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[C:22](Cl)(=[O:30])[O:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.N1C=CC=CC=1.O(C(C)C)C(C)C>O.ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([NH:21][C:22](=[O:30])[O:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=1

Komponenten

7

Edukt 4

HCID 1049PyridineHCID 7914Diisopropyl EtherHCID 15891Phenyl chloroformateHCID 154406Benzenamine, 4-(4-(4-methoxyphenyl)-1-piperazinyl)-

Produkt 1

HCID 981607Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamateAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 6 parts of 4-[4-(4-methoxyphenyl)-1-piperazinyl]benzenamine, 3.6 parts of phenyl carbonochloridate, 75 parts of pyridine and 98 parts of dichloromethane was stirred and warmed till all solid entered solution. Stirring was continued for 30 minutes at room temperature. The reaction mixture was poured into 500 parts of water and 210 parts of 2,2'-oxybispropane were added. The whole was stirred for a while. The precipitated product was filtered off and crystallized from 1-butanol, yielding 5.2 parts (61%) of phenyl [4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate; mp. 204.5 (intermediate 18).

Aufarbeitung

  1. temperaturewarmed till all solid
  2. stirringStirring
  3. additionwere added
  4. stirringThe whole was stirred for a while
  5. filtrationThe precipitated product was filtered off
  6. customcrystallized from 1-butanol

Quellen und Nachweise

ORD-Eintrag
ord-7e34742856264106811cee026c524991
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04791111

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