Hydrochloric Acid → 6-Methoxy-7-(3-methylsulphonylpropoxy)-3,4-dihydroquinazolin-4-one

HRID 454058

Reaktionsgleichung

Reaktionsgleichung von HRID 454058
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH2:14][CH2:15][CH2:16][S:17]([CH3:20])(=[O:19])=[O:18])[N:9]=[CH:8][N:7](COC(=O)C(C)(C)C)[C:6]2=[O:29].[OH-].[Na+].CC1C=CC(COC(NNC(C2C=NC=CN=2)=O)=O)=CC=1.Cl>CO.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH2:14][CH2:15][CH2:16][S:17]([CH3:20])(=[O:19])=[O:18])[N:9]=[CH:8][NH:7][C:6]2=[O:29]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 478568p-tolylmethyl N-(pyrazine-2-carbonylamino)carbamateHCID 220305896-Methoxy-7-(3-methylsulphonylpropoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one

Produkt 1

HCID 1357631126-Methoxy-7-(3-methylsulphonylpropoxy)-3,4-dihydroquinazolin-4-oneAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

6-Methoxy-7-(3-methylsulphonylpropoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (7 g, 17 mmol) was suspended in methanol and 2M sodium hydroxide (3.3 ml, 6.6 mmol) was added with continuous stirring. The reaction mixture became homogeneous after 15 minutes. After a further 45 minutes water was added (7 ml) and the reaction mixture was adjusted to pH10 with 2M hydrochloric acid. The precipitate (a white solid) was collected by filtration, washed with water and dried over phosphorus pentoxide under vacuum to give 6-methoxy-7-(3-methylsulphonylpropoxy)-3,4-dihydroquinazolin-4-one (5g, 90%).

Aufarbeitung

  1. filtrationThe precipitate (a white solid) was collected by filtration
  2. washwashed with water
  3. dry with materialdried over phosphorus pentoxide under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4bf681d41ebc43bbaeb5daa86166a889
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08492560B2

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