Acetic Acid → HCID 67250894、化合物

HRID 410388ノート

反応式

HRID 410388 の反応式
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][N:3]=1.[Br:10][C:11]1[CH:12]=[C:13]([CH:15]=[C:16]([CH3:18])[CH:17]=1)[NH2:14].C(O)(=O)C>O1CCOCC1>[Br:10][C:11]1[CH:12]=[C:13]([NH:14][C:2]2[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][N:3]=2)[CH:15]=[C:16]([CH3:18])[CH:17]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 5889352-Chloro-4-methoxypyrimidineHCID 30185263-Bromo-5-methylaniline

生成物 1

HCID 67250894HCID 67250894、化合物収率 100%

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

A 10-20 mL microwave vial was charged with 2-chloro-4-methoxypyrimidine (0.835 g, 5.78 mmol), 3-bromo-5-methylaniline (1.075 g, 5.78 mmol), acetic acid (0.347 mL, 6.06 mmol) and dioxane (11.55 mL). The system was purged and flushed with Ar(g) three times before sealing and heating to 120° C. for 3 hours. The mixture was cooled and stirred overnight. The light brown solids were collected by filtration and were dried in a vacuum oven overnight to yield N-(3-bromo-5-methylphenyl)-4-methoxypyrimidin-2-amine (1.7 g, 5.78 mmol, 100% yield) as a tan solid. MS ESI: [M+H]+ m/z 296.0.

後処理

  1. customThe system was purged
  2. customflushed with Ar(g) three times
  3. temperatureThe mixture was cooled
  4. filtrationThe light brown solids were collected by filtration
  5. customwere dried in a vacuum oven overnight

出典と根拠

ORDレコード
ord-842358daa5af4a84a723a68096a3efff
出典データセット
uspto-grants-2014_06
特許番号
US08759366B2

反応ノート

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