Sodium Hydroxide → HCID 46245197, Verbindung

HRID 1846571Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1846571
Cl.[NH:2]1[C:7]2[N:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2([CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[O:4][C:3]1=[O:17].Cl[C:19]1[N:24]=[CH:23][N:22]=[C:21]([O:25][C:26]2[CH:27]=[C:28]([CH3:39])[C:29]3[N:33]=[C:32]([CH2:34][CH2:35][O:36][CH3:37])[NH:31][C:30]=3[CH:38]=2)[CH:20]=1.CCN(C(C)C)C(C)C.[OH-].[Na+]>CN(C=O)C>[CH3:37][O:36][CH2:35][CH2:34][C:32]1[NH:31][C:30]2[CH:38]=[C:26]([O:25][C:21]3[N:22]=[CH:23][N:24]=[C:19]([N:14]4[CH2:13][CH2:12][C:5]5([O:4][C:3](=[O:17])[NH:2][C:7]6[N:8]=[CH:9][CH:10]=[CH:11][C:6]5=6)[CH2:16][CH2:15]4)[CH:20]=3)[CH:27]=[C:28]([CH3:39])[C:29]=2[N:33]=1

Komponenten

6

Edukt 4

HCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 66687106Spiro[piperidine-4,4'-pyrido[2,3-d][1,3]oxazin]-2'(1'H)-one hydrochlorideHCID 86663934HCID 86663934, Verbindung

Produkt 1

HCID 46245197HCID 46245197, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

29 mg (0.11 mmol) spiro[piperidin-4,4′-pyrido[2,3-d][1,3]oxazin]-2′(1′H)-one hydrochloride, 29 mg (0.09 mmol) 6-(6-chloropyrimidin-4-yloxy)-2-(2-methoxyethyl)-4-methyl-1H-benzo-[d]imidazole and 50 μL (0.39 mmol) DIPEA in 2.0 mL DMF were stirred overnight at 50° C. The reaction mixture was purified by chromatography. The fractions containing product were combined and evaporated down i.vac. to leave the aqueous residue. This was neutralised with a 1M aqueous NaOH solution. The precipitate formed was suction filtered, washed and dried.

Aufarbeitung

  1. customThe reaction mixture was purified by chromatography
  2. additionThe fractions containing product
  3. customevaporated down i.vac
  4. customto leave the aqueous residue
  5. customThe precipitate formed
  6. filtrationfiltered
  7. washwashed
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-fbe32ae09f04453d9fd5f0f1f3121050
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08952014B2

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