Hydrochloric Acid → 1-{4-[(2H-1,3-benzodioxol-5-ylmethyl)amino]-6-chloroquinazolin-2-yl}piperidine-4-carboxylic acid hydrochloride

HRID 1900692

Reaktionsgleichung

Reaktionsgleichung von HRID 1900692
[C:1]([CH:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]([NH:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]4[O:28][CH2:29][O:30][C:24]=4[CH:23]=3)[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([Cl:31])[CH:16]=3)[N:11]=2)[CH2:6][CH2:5]1)([OH:3])=[O:2].Cl>O1CCCC1.C(O)C>[ClH:31].[C:1]([CH:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:19]=[C:18]([NH:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]4[O:28][CH2:29][O:30][C:24]=4[CH:23]=3)[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([Cl:31])[CH:16]=3)[N:11]=2)[CH2:6][CH2:5]1)([OH:3])=[O:2]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 53114861-(6-Chloro-4-(3,4-methylenedioxybenzyl)aminoquinazolin-2-yl)piperidine-4-carboxylic acid

Produkt 1

HCID 211839871-{4-[(2H-1,3-benzodioxol-5-ylmethyl)amino]-6-chloroquinazolin-2-yl}piperidine-4-carboxylic acid hydrochlorideAusbeute 172,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

2.00 g (4.54 mmol) of the 2-(4-carboxy-piperidino)-4-(3,4-methylenedioxybenzylamino)-6-chloroquinazoline prepared in Example 222 was dissolved in a mixture comprising 25 ml of tetrahydrofuran and 25 ml of ethanol under heating, followed by the dropwise addition of 1.0 ml of an 8M ethanolic solution of hydrochloric acid. The obtained mixture was cooled by allowing to stand to precipitate crystals. The crystals were recovered by filtration, washed with tetrahydrofuran, and air-dried to give 1.87 g of the title compound.

Aufarbeitung

  1. temperatureunder heating
  2. temperatureThe obtained mixture was cooled
  3. customto precipitate crystals
  4. filtrationThe crystals were recovered by filtration
  5. washwashed with tetrahydrofuran
  6. customair-dried

Quellen und Nachweise

ORD-Eintrag
ord-d0e4aa5a3f75414bb53fa265afda8f3d
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05576322

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