Hydrochloric Acid → 2-Chloro-4-(2,5-dichloroanilino)pyrimidine

HRID 347742

反応式

HRID 347742 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[Cl:9][C:10]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:11]=1[NH2:12].Cl>C(O)CCC>[Cl:1][C:2]1[N:7]=[C:6]([NH:12][C:11]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:10]=2[Cl:9])[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 72622,5-DichloroanilineHCID 775312,4-Dichloropyrimidine

生成物 1

HCID 179811312-Chloro-4-(2,5-dichloroanilino)pyrimidine収率 20%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

2,4-Dichloropyrimidine (50 g, 0.34 mol), 2,5-dichloroaniline (54.38 g, 0.34 mol) and concentrated hydrochloric acid (cat. amount) were dissolved in n-butanol (250 ml). The reaction mixture was stirred at room temperature for 12 hours after which the solid that had formed was collected by filtration. The organics were allowed to stand for 48 hours and the solid that formed was collected by filtration, washed with EtOAc and dried to give the title product as a white solid (18.65 g). NMR (300 MHz): 6.82 (d, 1H), 7.31 (dd, 1H), 7.58 (d, 1H), 7.82 (s, 1H), 8.19 (d, 1H), 9.82 (s, 1H); m/z: (ES+) 273.9 (MH+).

後処理

  1. customthat had formed
  2. filtrationwas collected by filtration
  3. waitto stand for 48 hours
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. washwashed with EtOAc
  7. customdried

出典と根拠

ORDレコード
ord-44c263d9e5d5409fb10eec7b770bee1f
出典データセット
uspto-grants-2007_02
特許番号
US07176212B2

関連ノート

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