Sodium Hydroxide → 3-(1-carboxy-3-phenylpropylamino)-5-carboxymethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

HRID 1719118Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1719118
C([O:3][C:4]([CH:6]([NH:15][CH:16]1[C:22](=[O:23])[N:21]([CH2:24][C:25]([O:27]CC)=[O:26])[C:20]2[CH:30]=[CH:31][CH:32]=[CH:33][C:19]=2[S:18][CH2:17]1)[CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[C:4]([CH:6]([NH:15][CH:16]1[C:22](=[O:23])[N:21]([CH2:24][C:25]([OH:27])=[O:26])[C:20]2[CH:30]=[CH:31][CH:32]=[CH:33][C:19]=2[S:18][CH2:17]1)[CH2:7][CH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)([OH:5])=[O:3]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 134744743-(1-ethoxycarbonyl-3-phenylpropylamino)-5-ethoxycarbonylmethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

Produkt 1

HCID 133751243-(1-carboxy-3-phenylpropylamino)-5-carboxymethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-oneAusbeute 61,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1.2 g of 3-(1-ethoxycarbonyl-3-phenylpropylamino)-5-ethoxycarbonylmethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one was dissolved in 15 ml of ethanol, and 6 ml of 1N NaOH was added thereto. The resulting mixture was stirred at room temperature, so that white crystals were precipitated. After 1.5 hours, the ethanol was distilled off under reduced pressure and water was added to the residue. After a small amount of insoluble matter was filtered off, the filtrate was adjusted to pH 3-4 with 6N hydrochloric acid. The precipitated crystals were separated by filtration and washed with cold water and then with ether to obtain 650 mg of the desired compound.

Aufarbeitung

  1. customwere precipitated
  2. distillationthe ethanol was distilled off under reduced pressure and water
  3. additionwas added to the residue
  4. filtrationAfter a small amount of insoluble matter was filtered off
  5. customThe precipitated crystals were separated by filtration
  6. washwashed with cold water

Quellen und Nachweise

ORD-Eintrag
ord-f353b51500464d3a944c722b68f26198
Quelldatensatz
uspto-grants-1985_09
Patentnummer
US04539150

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