Acetic Acid → HCID 67248097、化合物

HRID 410567

反応式

HRID 410567 の反応式
C(O)(=O)C.Cl[C:6]1[N:11]=[C:10]([CH:12]([CH3:14])[CH3:13])[CH:9]=[CH:8][N:7]=1.[Br:15][C:16]1[CH:17]=[C:18]([CH:20]=[C:21]([CH3:23])[CH:22]=1)[NH2:19]>O1CCOCC1>[Br:15][C:16]1[CH:17]=[C:18]([NH:19][C:6]2[N:11]=[C:10]([CH:12]([CH3:14])[CH3:13])[CH:9]=[CH:8][N:7]=2)[CH:20]=[C:21]([CH3:23])[CH:22]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 30185263-Bromo-5-methylanilineHCID 249019162-Chloro-4-(propan-2-yl)pyrimidine

生成物 1

HCID 67248097HCID 67248097、化合物収率 98.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

Acetic acid (0.192 mL, 3.35 mmol) was added to commercially available 2-chloro-4-(propan-2-yl)pyrimidine (0.5 g, 3.19 mmol) and 3-bromo-5-methylaniline (0.900 g, 3.19 mmol) suspended in dioxane (6.39 mL). Reaction was heated to 120° C. (bath temp) overnight. Then, the reaction was cooled to room temperature and purified by column chromatography on silica gel eluting with ethyl acetate and hexanes to give N-(3-bromo-5-methylphenyl)-4-(propan-2-yl)-pyrimidin-2-amine (959.8 mg, 3.13 mmol, 98%) as a white solid.

後処理

  1. customReaction
  2. temperatureThen, the reaction was cooled to room temperature
  3. custompurified by column chromatography on silica gel eluting with ethyl acetate and hexanes

出典と根拠

ORDレコード
ord-6f0a6f8c243e448aacaf35fdaef543d9
出典データセット
uspto-grants-2014_06
特許番号
US08759366B2

関連ノート

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