Sulfuric Acid → HCID 136410984、化合物

HRID 1626316ノート

反応式

HRID 1626316 の反応式
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

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 86670632HCID 86670632、化合物

生成物 1

HCID 136410984HCID 136410984、化合物収率 72%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8ace9524f97240979c1dd2991e8a99b2
出典データセット
uspto-grants-2014_07
特許番号
US08785453B2

反応ノート

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