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

HRID 2351088ノート

反応式

HRID 2351088 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d5cfc8e65e5e45c1bd812405d8b4536c
出典データセット
uspto-grants-1989_10
特許番号
US04871841

反応ノート

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