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

HRID 2222280ノート

反応式

HRID 2222280 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2c166629aba74578a74367b6725b4103
出典データセット
uspto-grants-2008_05
特許番号
US07371769B2

反応ノート

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