Sulfuric Acid → HCID 136410984, 화합물

HRID 1626316노트

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HRID 1626316 반응식
Cl[C:2]1[C:7]([NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:5]=[CH:4][N:3]=1.S(=O)(=O)(O)[OH:25].C([O-])(O)=O.[Na+]>CC(O)C>[C:10]1([C:9]2[N:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:6]3[N:5]=[CH:4][NH:3][C:2](=[O:25])[C:7]=3[N:8]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 86670632HCID 86670632, 화합물

생성물 1

HCID 136410984HCID 136410984, 화합물수율 72%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
90 °C

실험 절차

To a stirred solution of N-(4-chloro-6-(phenylamino)pyrimidin-5-yl)benzamide obtained in step 2 (35 g, 108 mmol) in 2-propanol (360 mL) was added sulfuric acid (18.2 mL, 323.3 mmol) at 0° C. The reaction mixture was heated to reflux at 90° C. overnight. After cooled to room temperature NaHCO3 (aq) was added to the resulting reaction mixture and stirred. The resulting mixture was filtered with water (600 mL). The collected solid was dried under reduced pressure to obtain the title compound (22.3 g, 72%) as white solid.

후처리

  1. temperatureThe reaction mixture was heated
  2. additionwas added to the resulting reaction mixture
  3. filtrationThe resulting mixture was filtered with water (600 mL)
  4. customThe collected solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-8ace9524f97240979c1dd2991e8a99b2
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785453B2

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