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

HRID 1245419
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HRID 1245419 반응식
[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
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참가 물질

6

반응물 3

HCID 78124-ChloroanilineHCID 81531DiisopropylethylamineHCID 21912455HCID 21912455, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 312751,4-Dioxane용매

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온도
110 °C

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-8f40eacb5a7e497b877b45bf4af7c22d
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07125881B2

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