Formic Acid → 1,4-Benzoxazepine-4(5H)-carboxaldehyde, 2,3-dihydro-

HRID 429728Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 429728
[CH:1](O)=[O:2].C(OC(=O)C)(=O)C.[O:11]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[CH2:15][NH:14][CH2:13][CH2:12]1>ClCCl>[CH:1]([N:14]1[CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:11][CH2:12][CH2:13]1)=[O:2]

Komponenten

5

Edukt 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 218827752,3,4,5-Tetrahydro-1,4-benzoxazepine

Produkt 1

HCID 118195761,4-Benzoxazepine-4(5H)-carboxaldehyde, 2,3-dihydro-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To 15 ml of formic acid was added dropwise 5 ml of acetic anhydride, and the mixture was stirred for 20 minutes at room temperature. To the mixture was added dropwise a solution of 2.2 g of 2,3,4,5-tetrahydro-1,4-benzoxazepine in 10 ml of dichloromethane, and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was poured into ice-water, then the mixture was subjected to extraction with dichloromethane. The extract was washed successively with a saturated aqueous solution of sodium bicarbonate, and water. The mixture was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give 2.6 g of 4-formyl-2,3,4,5-tetrahydro-1,4-benzoxazepine as an oily anhydrous substance.

Aufarbeitung

  1. stirringthe mixture was stirred for 30 minutes at room temperature
  2. extractionthe mixture was subjected to extraction with dichloromethane
  3. washThe extract was washed successively with a saturated aqueous solution of sodium bicarbonate, and water
  4. dry with materialThe mixture was dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9284ce5b04994460b5307cfedaf51903
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06319916B1

Notizen zur Reaktion

Wird geladen…