Sodium Iodide → R 47243

HRID 1761501

Reaktionsgleichung

Reaktionsgleichung von HRID 1761501
Br[CH2:2][CH:3]1[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1.Br.Br.[NH:15]1[CH2:20][CH2:19][CH:18]([CH2:21][NH:22][C:23]2[S:24][C:25]3[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=3[N:27]=2)[CH2:17][CH2:16]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>O.CN(C)C=O>[O:8]1[C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4][CH:3]1[CH2:2][N:15]1[CH2:20][CH2:19][CH:18]([CH2:21][NH:22][C:23]2[S:24][C:25]3[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=3[N:27]=2)[CH2:17][CH2:16]1

Komponenten

7

Edukt 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 983332-Bromomethyl-1,4-benzodioxaneHCID 14048948N-(4-piperidinylmethyl)-2-benzothiazolamine dihydrobromide

Produkt 1

HCID 128556R 47243

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 3.8 parts of 2-(bromomethyl)-2,3-dihydro-1,4-benzodioxin, 6.3 parts of N-(4-piperidinylmethyl)-2-benzothiazolamine dihydrobromide, 10 parts of sodium carbonate, 0.1 parts of sodium iodide and 68 parts of N,N-dimethylformamide was stirred for 48 hours at 70° C. The reaction mixture was poured into water and the product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The oily residue was crystallized from acetonitrile, yielding 2.8 parts of N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]methyl]-2-benzothiazolamine; mp. 139.9° C. (compound 1).

Aufarbeitung

  1. extractionthe product was extracted with 4-methyl-2-pentanone
  2. customThe extract was dried
  3. filtrationfiltered
  4. customevaporated
  5. customThe oily residue was crystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-b0d67e3a6f1d44e18e0f115a0542dbc9
Quelldatensatz
uspto-grants-1989_05
Patentnummer
US04826848

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