Dimethylformamide → 6-bromo-2-methylpyrazolo[1,5-a]pyrimidine-3-carbaldehyde

HRID 2043576ノート

反応式

HRID 2043576 の反応式
O=P(Cl)(Cl)Cl.[Br:6][C:7]1[CH:8]=[N:9][C:10]2[N:11]([N:13]=[C:14]([CH3:16])[CH:15]=2)[CH:12]=1.CN([CH:20]=[O:21])C>>[Br:6][C:7]1[CH:8]=[N:9][C:10]2[N:11]([N:13]=[C:14]([CH3:16])[C:15]=2[CH:20]=[O:21])[CH:12]=1

参加物

4

反応物 3

HCID 6228Dimethylformamide2 回HCID 24813Phosphorus oxychlorideHCID 159800416-Bromo-2-methylpyrazolo[1,5-a]pyrimidine

生成物 1

HCID 170961496-bromo-2-methylpyrazolo[1,5-a]pyrimidine-3-carbaldehyde収率 59%

反応条件

温度
0 °C

実験手順

POCl3 (1.84 mmol, 1.3 eq, 172 μl) is added dropwise to DMF (1 ml) at 0° C. and the resulting solution is stirred at 0° C. during 30 minutes. Then, a solution of 6-bromo-2-methylpyrazolo[1,5-a]pyrimidine x14 (1.415 mmol, 1 eq, 300 mg) in DMF (1 ml) is added and the mixture is stirred for 30 minutes at room temperature. The reaction is quenched with water (100 ml). The resulting solid is filtered and washed with water to give 200 mg of 6-bromo-2-methylpyrazolo[1,5-a]pyrimidine-3-carbaldehyde x21 as a solid.

後処理

  1. stirringthe mixture is stirred for 30 minutes at room temperature
  2. customThe reaction is quenched with water (100 ml)
  3. filtrationThe resulting solid is filtered
  4. washwashed with water

出典と根拠

ORDレコード
ord-08596b8181794189927a01188dc26284
出典データセット
uspto-grants-2013_11
特許番号
US08586623B2

反応ノート

読み込み中…