Carbon Dioxide → 5-Chloro-2-(methylthio)pyrimidine

HRID 1413043ノート

反応式

HRID 1413043 の反応式
[Cl:1][C:2]1[C:3](C(O)=O)=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.C(=O)=O>>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1

参加物

3

反応物 2

HCID 280Carbon DioxideHCID 7257115-Chloro-2-(methylsulfanyl)pyrimidine-4-carboxylic acid

生成物 1

HCID 47370635-Chloro-2-(methylthio)pyrimidine収率 89.2%

実験手順

5-Chloro-2-methylthio-4-pyrimidine carboxylic acid (30 g) was heated at 180°-200° C. until all the solid had melted and the evolution of carbon dioxide had ceased (5 min). The residue was allowed to cool and then washed with several portions of chloroform. The chloroform washings were filtered to remove dark insoluble material and the filtrate was concentrated to give 5-chloro-2-methylthiopyrimidine as a pale brown crystalline solid (21 g, 89%), m.p. 55° C.

後処理

  1. custom(5 min)
  2. temperatureto cool
  3. washwashed with several portions of chloroform
  4. filtrationThe chloroform washings were filtered
  5. customto remove dark insoluble material
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-97f3674f964e4f6c8af28d78938cc3ec
出典データセット
uspto-grants-1981_02
特許番号
US04248618

反応ノート

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