Phosgene → 8-chlorodibenz[b,f][1,4]thiazepine-10(11H)-carbonyl chloride

HRID 1707650Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1707650
[C:1]([Cl:4])(Cl)=[O:2].[Cl:5][C:6]1[CH:20]=[CH:19][C:9]2[S:10][C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][NH:14][C:8]=2[CH:7]=1.C(N(CC)CC)C>O1CCCC1>[Cl:5][C:6]1[CH:20]=[CH:19][C:9]2[S:10][C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][N:14]([C:1]([Cl:4])=[O:2])[C:8]=2[CH:7]=1

Komponenten

5

Edukt 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 542201108-Chloro-10,11-dihydrodibenzo[b,f][1,4]thiazepine

Produkt 1

HCID 229217168-chlorodibenz[b,f][1,4]thiazepine-10(11H)-carbonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a cold (ice-H2O bath), stirred solution of phosgene (1.93M in toluene; 8.6 mL) in anhydrous tetrahydrofuran (40 mL) under a nitrogen atmosphere is added, dropwise, a solution of the product of Example 104 (8-chloro-10,11-dihydrodibenzo[b,f][1,4]thiazepine) (2.00 g) and triethylamine (1.3 mL) in anhydrous tetrahydrofuran (30 mL). The resulting mixture is stirred at room temperature for 90 minutes, and the solvent is then evaporated in vacuo to provide the title product.

Aufarbeitung

  1. additionis added
  2. customthe solvent is then evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a7791d8f8ad94dac93a51d96ca426dcc
Quelldatensatz
uspto-grants-1994_10
Patentnummer
US05354747

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