Ammonia → HCID 16426513, 화합물

HRID 2206843노트

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HRID 2206843 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 16426513HCID 16426513, 화합물수율 53%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

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온도
5 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-0c7c34a76b774d5ea75187e804e921d9
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09375002B2

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