Pyridine → 2-methylthio-5-(2-chloroethyl)-3,6-dimethyl-3H-pyrimidin-4-one

HRID 2222280노트

반응식

HRID 2222280 반응식
[CH3:1][S:2][C:3]1[N:8]([CH3:9])[C:7](=[O:10])[C:6]([CH2:11][CH2:12]O)=[C:5]([CH3:14])[N:4]=1.N1C=CC=CC=1.S(Cl)([Cl:23])=O>C(Cl)(Cl)Cl>[CH3:1][S:2][C:3]1[N:8]([CH3:9])[C:7](=[O:10])[C:6]([CH2:11][CH2:12][Cl:23])=[C:5]([CH3:14])[N:4]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 693142522-methylthio-5-(2-hydroxyethyl)-3,6-dimethyl-3H-pyrimidin-4-one

생성물 1

HCID 693164112-methylthio-5-(2-chloroethyl)-3,6-dimethyl-3H-pyrimidin-4-one

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 2-methylthio-5-(2-hydroxyethyl)-3,6-dimethyl-3H-pyrimidin-4-one (20.3 g, 0.095 mol) in chloroform (200 ml) was added one equivalent of pyridine (7.6 ml), followed by slow addition of three equivalents of thionyl chloride (21 ml). After stirring for 15 minutes, the mixture was concentrated and water (300 ml) was added. The precipitate was collected and washed with water, isopropyl alcohol and petroleum ether. Yield 34.4 g (64%). Yield 20.3 g (92%). Mp. 135-137° C.

후처리

  1. concentrationthe mixture was concentrated
  2. additionwater (300 ml) was added
  3. customThe precipitate was collected
  4. washwashed with water, isopropyl alcohol and petroleum ether

출처 및 근거

ORD 기록
ord-2c166629aba74578a74367b6725b4103
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07371769B2

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