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Diisopropylethylamine → (4-Chloro-6-{N'-[1-(4-trifluoromethoxyphenyl)-methylidene]-hydrazino}-[1,3,5]triazin-2-yl)-(4-fluoro-3-trifluoromethylphenyl)-amine

HRID 563851
ノート
印刷プレビュー

反応式

HRID 563851 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([C:17]([F:20])([F:19])[F:18])[CH:11]=2)[N:3]=1.C(N(C(C)C)CC)(C)C.[F:30][C:31]([F:43])([F:42])[O:32][C:33]1[CH:38]=[CH:37][C:36]([CH:39]=[N:40][NH2:41])=[CH:35][CH:34]=1>O1CCOCC1>[Cl:8][C:6]1[N:7]=[C:2]([NH:41][N:40]=[CH:39][C:36]2[CH:35]=[CH:34][C:33]([O:32][C:31]([F:30])([F:43])[F:42])=[CH:38][CH:37]=2)[N:3]=[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([C:17]([F:20])([F:19])[F:18])[CH:11]=2)[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 57507188(4,6-Dichloro-[1,3,5]triazin-2-yl)-(4-fluoro-3-trifluoromethylphenyl)amineHCID 66679788[1-(4-Trifluoromethoxyphenyl)-methylidene]-hydrazine

生成物 1

HCID 76550911(4-Chloro-6-{N'-[1-(4-trifluoromethoxyphenyl)-methylidene]-hydrazino}-[1,3,5]triazin-2-yl)-(4-fluoro-3-trifluoromethylphenyl)-amine収率 67%

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

4,6-Dichloro-N-(3-trifluoromethyl-4-fluorophenyl)-1,3,5-triazine-2-amine (XVII) (2.0 g, 6.2 mmol) was dissolved in dioxane (40 mL). Diisopropylethylamine (1.6 mL, 9.32 mmol) was added followed by [4-(trifluoromethoxy)benzylidene]hydrazine (XX) (1.3 g, 6.2 mmol). The reaction was stirred at room temperature overnight. The solvent was removed under vacuum, and the residue diluted with ethyl ether (25 mL). The organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated to a yellow powder. This powder was washed with acetonitrile to give {4-chloro-6-[N′-(4-trifluoromethoxybenzylidene)hydrazino]-1,3,5-triazin-2-yl}-(4-fluoro-3-trifluoromethylphenyl)-amine (XXI) as a white solid; (2.1 g, 67% yield): m.p. 109-111° C.; 1H NMR (CDCl3): δ 8.9, (bs, 1H); 8.5 (bs, 1H); 7.95 (s, 1H); 7.75 (bs, 2H); 7.45 (bs, 1H); 7.24 (m, 4H); ESI/MS 494 (M+H).

後処理

  1. customThe solvent was removed under vacuum
  2. additionthe residue diluted with ethyl ether (25 mL)
  3. washThe organic phase was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to a yellow powder
  7. washThis powder was washed with acetonitrile

出典と根拠

ORDレコード
ord-01098b860824453e9415749440257d10
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067588B2

反応ノート

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