Acetic Acid → HCID 67248097、化合物

HRID 1040057

反応式

HRID 1040057 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-isopropylpyrimidine

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-50cc06cacf6e42628e60dc22f68cdc50
出典データセット
uspto-grants-2013_10
特許番号
US08551984B2

関連ノート

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