Potassium Iodide → HCID 20360368, Verbindung

HRID 2082677Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2082677
Cl.Cl[CH2:3][CH2:4][NH:5][CH:6]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1.[Cl:21][C:22]1[CH:37]=[CH:36][C:25]2[N:26]([CH:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)[C:27](=[O:29])[NH:28][C:24]=2[CH:23]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[F:13][C:10]1[CH:11]=[CH:12][C:7]([CH:6]([NH:5][CH2:4][CH2:3][N:33]2[CH2:32][CH2:31][CH:30]([N:26]3[C:25]4[CH:36]=[CH:37][C:22]([Cl:21])=[CH:23][C:24]=4[NH:28][C:27]3=[O:29])[CH2:35][CH2:34]2)[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)=[CH:8][CH:9]=1

Komponenten

7

Edukt 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 1046075-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 3017749N-[Bis(4-fluorophenyl)methyl]-2-chloroethan-1-amine--hydrogen chloride (1/1)

Produkt 1

HCID 20360368HCID 20360368, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 7909Methyl Isobutyl KetoneLösungsmittel

Versuchsvorschrift

A mixture of 10 parts of N-(2-chloroethyl)-4-fluoro-α-(4-fluorophenyl)benzenemethanamine hydrochloride, 7.3 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 10.6 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. Water is added to the reaction mixture. The precipitated product is filtered off and set aside. From the filtrate, the organic phase is separated, washed with water, dried, filtered and evaporated. The residue is stirred in 4-methyl-2-pentanone. The solid product is filtered off, combined with the precipitated product, obtained above, and crystallized from 4-methyl-2-pentanone. The product is filtered off and dried in vacuo at 95° C, yielding 5 parts of 1-{1-[2-{[bis(4-fluorophenyl)methyl]amino}ethyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one; mp. 198.6° C.

Aufarbeitung

  1. temperaturerefluxed overnight
  2. filtrationThe precipitated product is filtered off
  3. customFrom the filtrate, the organic phase is separated
  4. washwashed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. stirringThe residue is stirred in 4-methyl-2-pentanone
  9. filtrationThe solid product is filtered off
  10. customobtained above, and
  11. customcrystallized from 4-methyl-2-pentanone
  12. filtrationThe product is filtered off
  13. customdried in vacuo at 95° C

Quellen und Nachweise

ORD-Eintrag
ord-d7bf29c4a1b442038f67a63a33954eef
Quelldatensatz
uspto-grants-1978_04
Patentnummer
US04082755

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