Benzyl chloroformate → (Tetrahydro-2-oxo-1(2H)-pyrimidinyl)carbamic acid, phenylmethyl ester

HRID 2351088Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2351088
Cl.[NH2:2][N:3]1[CH2:8][CH2:7][CH2:6][NH:5][C:4]1=[O:9].[CH2:10]([O:17][C:18](Cl)=[O:19])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O.O1CCCC1>[O:9]=[C:4]1[NH:5][CH2:6][CH2:7][CH2:8][N:3]1[NH:2][C:18](=[O:19])[O:17][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

Komponenten

5

Edukt 2

HCID 10387Benzyl chloroformateHCID 1317161453-Aminotetrahydro-2(1H)-pyrimidinone, monohydrochloride

Produkt 1

HCID 54188774(Tetrahydro-2-oxo-1(2H)-pyrimidinyl)carbamic acid, phenylmethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

3-Aminotetrahydro-2(1H)-pyrimidinone, monohydrochloride (30 g, 0.198 mol) was dissolved in a mixture of 240 ml water and 200 ml tetrahydrofuran. The pH was adjusted to 8.5 and benzylchloroformate (33.8 g, 0.198 mmol) was added dropwise while keeping the pH between 8 and 9. After the pH remained constant, the mixture was stirred for an additional hour. The tetrahydrofuran was removed in vacuo and the resulting crystals were filtered off with suction, triturated with ether and dried in vacuo. Yield 35.6 g, melting point 161°-163° C.

Aufarbeitung

  1. additionwas added dropwise
  2. customThe tetrahydrofuran was removed in vacuo
  3. filtrationthe resulting crystals were filtered off with suction
  4. customtriturated with ether
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d5cfc8e65e5e45c1bd812405d8b4536c
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04871841

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