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Trifluoroacetic acid → 3-{4-[(2-Aminoethyl)amino]-1,2,5-oxadiazol-3-yl}-4-(3-chloro-4-fluorophenyl)-1,2,4-oxadiazol-5(4H)-one hydrochloride

HRID 69776
ノート
印刷プレビュー

反応式

HRID 69776 の反応式
C([SiH](C(C)C)C(C)C)(C)C.FC(F)(F)C(O)=O.[Cl:18][C:19]1[CH:20]=[C:21]([N:26]2[C:30](=[O:31])[O:29][N:28]=[C:27]2[C:32]2[C:36]([NH:37][CH2:38][CH2:39][NH:40]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)=[N:35][O:34][N:33]=2)[CH:22]=[CH:23][C:24]=1[F:25]>>[ClH:18].[NH2:40][CH2:39][CH2:38][NH:37][C:36]1[C:32]([C:27]2[N:26]([C:21]3[CH:22]=[CH:23][C:24]([F:25])=[C:19]([Cl:18])[CH:20]=3)[C:30](=[O:31])[O:29][N:28]=2)=[N:33][O:34][N:35]=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

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 138754Silane, tris(1-methylethyl)-HCID 666063854-(3-Chloro-4-fluorophenyl)-3-(4-{[2-(tritylamino)ethyl]amino}-1,2,5-oxadiazol-3-yl)-1,2,4-oxadiazol-5(4H)-one

生成物 1

HCID 666059023-{4-[(2-Aminoethyl)amino]-1,2,5-oxadiazol-3-yl}-4-(3-chloro-4-fluorophenyl)-1,2,4-oxadiazol-5(4H)-one hydrochloride収率 197.7%

反応条件

温度
25 °C

実験手順

A premixed solution of triisopropylsilane (3.4 mL, 17 mmol) and trifluoroacetic acid (44 mL, 570 mmol) was added to 4-(3-chloro-4-fluorophenyl)-3-(4-{[2-(tritylamino)ethyl]amino}-1,2,5-oxadiazol-3-yl)-1,2,4-oxadiazol-5(4H)-one (6.5 g, 11 mmol) and the resulting suspension was stirred at 25° C. for 30 min. The reaction mixture was filtered and washed with trifluoroacetic acid. The filtrate was concentrated to an oil which was diluted with methanol (25 mL), cooled to 0° C., treated with 4 M HCl in 1,4-dioxane (14 mL), and stirred at 25° C. for 15 min. The mixture was concentrated to a solid that was treated with diethyl ether (50 mL) and filtered. The solid was washed with diethyl ether (50 mL) and dried to give the desired product (4.1 g, 98%) as a white solid. LCMS for C12H11ClFN6O3 (M+H)+: m/z=341.1. 1H NMR (300 MHz, DMSO-d6): δ 8.05-8.00 (m, 4 H), 7.75-7.69 (m, 1 H), 7.64 (dd, J=9.1, 8.8 Hz, 1 H), 6.77 (dd, J=5.9, 5.9 Hz, 1 H), 3.54-3.47 (m, 2 H), 3.04-2.99 (m, 2 H).

後処理

  1. filtrationThe reaction mixture was filtered
  2. washwashed with trifluoroacetic acid
  3. concentrationThe filtrate was concentrated to an oil which
  4. additionwas diluted with methanol (25 mL)
  5. temperaturecooled to 0° C.
  6. additiontreated with 4 M HCl in 1,4-dioxane (14 mL)
  7. stirringstirred at 25° C. for 15 min
  8. concentrationThe mixture was concentrated to a solid
  9. additionthat was treated with diethyl ether (50 mL)
  10. filtrationfiltered
  11. washThe solid was washed with diethyl ether (50 mL)
  12. customdried

出典と根拠

ORDレコード
ord-62264f9aab1043b88a7ef52e4f5ff1a9
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822511B2

反応ノート

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