4-Chloro-2-fluorobenzoyl chloride → HCID 21905770、化合物

HRID 1246791

反応式

HRID 1246791 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[C:3]=1[NH2:16].[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22](Cl)=[O:23])=[C:20]([F:27])[CH:19]=1>N1C=CC=CC=1.C(O)C>[Cl:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([NH:16][C:3]2[C:2]([Cl:1])=[N:7][CH:6]=[N:5][C:4]=2[NH:8][C:9]2[CH:10]=[CH:11][C:12]([Cl:15])=[CH:13][CH:14]=2)=[O:23])=[C:20]([F:27])[CH:19]=1

参加物

5

反応物 2

HCID 27736014-Chloro-2-fluorobenzoyl chlorideHCID 167263116-Chloro-N~4~-(4-chlorophenyl)pyrimidine-4,5-diamine

生成物 1

HCID 21905770HCID 21905770、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1049Pyridine溶媒

実験手順

6-Chloro-N4-(4-chlorophenyl)-pyrimidine-4,5-diamine I-(1A-1)a (6.6 g, 26 mmol) in pyridine (30 ml) was cooled to 0° C. and to it was added 4-chloro-2-fluorobenzoyl chloride (5 g, 26 mmol). The reaction was then allowed to warm to ambient temperature overnight. The heterogeneous reaction was diluted with ethanol (50 ml) and the resulting solid collected by filtration. The solids were slurried in toluene, which was then removed under reduced pressure to remove residual ethanol. The solid was slurried in diethyl ether and then collected by filtration to give I-(7A-91)a (8.3 g, 78%): +ACPI MS (M+1) 409.0; 1H NMR (400 MHz, CD3OD) δ 10.60 (s, 1H), 10.10 (s, 1H), 9.19 (s, 1H), 8.74 (t, J=8.1 Hz, 1H), 8.46–8.40 (m, 3H), 8.28 (dd, J=8.7, 2.1 Hz, 1H), 8.20 (d, J=8.7 Hz, 2H).

後処理

  1. customThe heterogeneous reaction
  2. filtrationthe resulting solid collected by filtration
  3. customwhich was then removed under reduced pressure
  4. customto remove residual ethanol
  5. filtrationcollected by filtration
  6. customto give I-(7A-91)a (8.3 g, 78%)

出典と根拠

ORDレコード
ord-1800146ac7c349e69101ea3ed85714e4
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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