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

HRID 2351088노트

반응식

HRID 2351088 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d5cfc8e65e5e45c1bd812405d8b4536c
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871841

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