Ammonia → HCID 16426513、化合物

HRID 2206843ノート

反応式

HRID 2206843 の反応式
[Cl:1][C:2]1[C:3]([C:10](Cl)=[O:11])=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.[NH3:13].O>O1CCOCC1.CO>[Cl:1][C:2]1[C:3]([C:10]([NH2:13])=[O:11])=[N:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1

参加物

6

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 140671885-Chloro-2-(methylsulfanyl)pyrimidine-4-carbonyl chloride

生成物 1

HCID 16426513HCID 16426513、化合物収率 53%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
5 °C

実験手順

15 g (67.2 mmol) of 5-chloro-2-(methylsulfanyl)pyrimidine-4-carbonyl chloride are dissolved in 35 ml of dioxane and cooled to 5° C. 57.3 g (0.4 mol) of 7N ammonia in methanol (about 12% strength solution) are slowly added dropwise to the cooled solution. During the addition, the reaction temperature was kept below 15° C. After the dropwise addition had ended, the reaction mixture was allowed to warm to room temperature and stirred for about 15 hours. The mixture was then added to water and the precipitated 5-chloro-2-(methylsulfanyl)pyrimidine-4-carboxamide was isolated (7.7 g, yield 53% at a purity of 95%).

後処理

  1. additionDuring the addition
  2. customwas kept below 15° C
  3. additionAfter the dropwise addition
  4. temperatureto warm to room temperature

出典と根拠

ORDレコード
ord-0c7c34a76b774d5ea75187e804e921d9
出典データセット
uspto-grants-2016_06
特許番号
US09375002B2

反応ノート

読み込み中…