Hydrochloric Acid → 6-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine

HRID 1246778

反応式

HRID 1246778 の反応式
[NH2:1][C:2]1[C:3]([Cl:9])=[N:4][CH:5]=[N:6][C:7]=1Cl.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1.Cl>O.C(O)C>[Cl:9][C:3]1[N:4]=[CH:5][N:6]=[C:7]([NH:15][C:14]2[CH:16]=[CH:17][C:11]([Cl:10])=[CH:12][CH:13]=2)[C:2]=1[NH2:1]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 78124-ChloroanilineHCID 794345-Amino-4,6-dichloropyrimidine

生成物 1

HCID 167263116-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine収率 99.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

5-amino-4,6-dichloropyrimidine (5.00 g, 29 mmol) and 4-chloroaniline (4.71 g, 36 mmol) were suspended in 80 ml H2O and 12 ml ethanol. Concentrated HCl (1.2 ml, 14.5 mmol) was added at room temperature followed by warming reaction to 82° C. After stirring for 19 hours the reaction was cooled to room temperature and stirred for 60 hours. The precipitate was collected on a sintered glass funnel and rinsed with water followed by hexanes. After drying under vacuum, I-(1A-1)a was obtained as an off-white solid (7.38 g, 98%): +ESI MS (M+1) 255.3; 1H NMR: (400 MHz, CD3OD): δ 7.87 (s, 1H), 7.66 (d, J=8.7 Hz, 2 H), 7.30 (d, J=8.7 Hz, 2 H).

後処理

  1. temperatureby warming
  2. customreaction to 82° C
  3. stirringstirred for 60 hours
  4. customThe precipitate was collected on a sintered glass funnel
  5. washrinsed with water
  6. customAfter drying under vacuum

出典と根拠

ORDレコード
ord-93a9f1f639764b5b8afb51c603527d38
出典データセット
uspto-grants-2006_10
特許番号
US07129239B2

関連ノート

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