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4-Chloroaniline → 5-chloro-N-(4-chlorophenyl)-2-fluoro-6-morpholin-4-ylpyrimidin-4-amine

HRID 1245419
ノート
印刷プレビュー

反応式

HRID 1245419 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[Cl:9][C:10]1[C:11]([N:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)=[N:12][C:13]([F:17])=[N:14][C:15]=1F.C(N(CC)C(C)C)(C)C>O1CCOCC1.C(O)(C)C>[Cl:9][C:10]1[C:15]([NH:6][C:5]2[CH:7]=[CH:8][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:14][C:13]([F:17])=[N:12][C:11]=1[N:18]1[CH2:23][CH2:22][O:21][CH2:20][CH2:19]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 78124-ChloroanilineHCID 81531DiisopropylethylamineHCID 21912455HCID 21912455、化合物

生成物 1

HCID 219124595-chloro-N-(4-chlorophenyl)-2-fluoro-6-morpholin-4-ylpyrimidin-4-amine

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

4-Chloroaniline (1.44 g) was added to a solution of the product from step (i) (0.88 g) and N,N-diisopropylethylamine (0.484 g) in 1,4-dioxane (15 ml) and isopropylalcohol (15 ml) and the mixture heated at 110° C. for 6 days. The mixture was partitioned between ethyl acetate and water, the organics dried (MgSO4), and evaporated under reduced pressure. The solid was triturated with ethyl acetate, filtered and the filtrate purified by chromatography on silica eluting with 3% ethyl acetate in toluene. Yield 0.28 g

後処理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. dry with materialthe organics dried (MgSO4)
  3. customevaporated under reduced pressure
  4. customThe solid was triturated with ethyl acetate
  5. filtrationfiltered
  6. customthe filtrate purified by chromatography on silica eluting with 3% ethyl acetate in toluene

出典と根拠

ORDレコード
ord-8f40eacb5a7e497b877b45bf4af7c22d
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07125881B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート