Dichloromethane → HCID 22990144, Verbindung

HRID 1169468Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1169468
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11](=[O:13])(=[O:12])[CH2:10][CH2:9][C:8]([C:14]([O:16][CH3:17])=[O:15])=[CH:7][C:6]=2[CH:18]=1.[CH2:19]([O:22][C:23]1[CH:24]=[C:25](OB(O)O)[CH:26]=[CH:27][CH:28]=1)[CH2:20][CH3:21].ClCCl>C(N(CC)CC)C>[CH2:19]([O:22][C:23]1[CH:28]=[C:27]([CH:26]=[CH:25][CH:24]=1)[O:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11](=[O:13])(=[O:12])[CH2:10][CH2:9][C:8]([C:14]([O:16][CH3:17])=[O:15])=[CH:7][C:6]=2[CH:18]=1)[CH2:20][CH3:21]

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 22989977Methyl 7-hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylateHCID 22989983HCID 22989983, Verbindung

Produkt 1

HCID 22990144HCID 22990144, VerbindungAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To a mixture of methyl 7-hydroxy-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (400 mg), 3-propoxyphenylboric acid (536 mg), cupric acetate (271 mg), MS 4A (0.8 g) and dichloromethane (15 ml) was added at room temperature triethylamine (1.04 ml), and the resulting mixture was stirred for 17 hours. The reaction mixture was filtered to remove an insoluble material and the filtrate was concentrated under reduced pressure. The residue was subjected to separation and purification using column chromatography (ethyl acetate:hexane 1:2) to obtain methyl 7-(3-propoxyphenoxy)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.39 g) as a light yellow, oily substance.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. customto remove an insoluble material
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was subjected to separation and purification

Quellen und Nachweise

ORD-Eintrag
ord-3bc26313c01243aab813975a823a428c
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06627651B1

Notizen zur Reaktion

Wird geladen…