2,3-Dichlorobenzaldehyde → HCID 15035858, Verbindung

HRID 1461474Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1461474
[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13](=O)[CH2:12][S:11](=[O:17])(=[O:16])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:18][C:19]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=O.[NH2:28]/[C:29](/[CH3:36])=[CH:30]\[C:31]([O:33][CH2:34][CH3:35])=[O:32]>C(O)C>[Cl:18][C:19]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]1[C:12]2[S:11](=[O:17])(=[O:16])[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:14][C:13]=2[NH:28][C:29]([CH3:36])=[C:30]1[C:31]([O:33][CH2:34][CH3:35])=[O:32]

Komponenten

5

Edukt 3

HCID 357452,3-DichlorobenzaldehydeHCID 6437562-Butenoic acid, 3-amino-, ethyl ester, (2Z)-HCID 19980844tert-Butyl 6-oxo-1,4-thiazepane-4-carboxylate 1,1-dioxide

Produkt 1

HCID 15035858HCID 15035858, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 4-N-(t-butyloxycarbonyl)-1,1-dioxo -2,3,4,5,6,7-hexahydro-1,4-thiazepin-6-one (2.00 g, 7.60 mmole) from Example 6, 2,3-dichlorobenzaldehyde (1.33 g, 7.60 mmole) and ethyl 3-aminocrotonate (0.98 g, 7.60 mmole) was heated to reflux in 40 mL of ethanol for 24 hours. The ethanol was removed under reduced pressure and replaced with 85 mL of toluene. The mixture was heated to reflux for 2 hours, cooled to room temperature and filtered to obtain the produce (2.45 g, 61%).

Aufarbeitung

  1. temperaturewas heated
  2. customThe ethanol was removed under reduced pressure
  3. temperatureThe mixture was heated
  4. temperatureto reflux for 2 hours
  5. filtrationfiltered
  6. customto obtain the
  7. customproduce (2.45 g, 61%)

Quellen und Nachweise

ORD-Eintrag
ord-06de9772ec26415da65775a0f59258d3
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05075440

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