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Hydrochloric Acid → 6-(3,5-difluorophenyl)-2-[(3-{1-[4-(morpholin-4-ylcarbonyl)phenyl]-1H-1,2,3-triazol-4-yl}-1H-indazol-5-yl)methyl]pyridazin-3(2H)-one

HRID 1520064
ノート
印刷プレビュー

反応式

HRID 1520064 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH2:16][C:17]3[CH:18]=[C:19]4[C:23](=[CH:24][CH:25]=3)[NH:22][N:21]=[C:20]4[C:26]3[N:27]=[N:28][N:29]([C:31]4[CH:39]=[CH:38][C:34]([C:35](O)=[O:36])=[CH:33][CH:32]=4)[CH:30]=3)[N:10]=2)[CH:5]=[C:6]([F:8])[CH:7]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.[NH:52]1[CH2:57][CH2:56][O:55][CH2:54][CH2:53]1.Cl>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([CH2:16][C:17]3[CH:18]=[C:19]4[C:23](=[CH:24][CH:25]=3)[NH:22][N:21]=[C:20]4[C:26]3[N:27]=[N:28][N:29]([C:31]4[CH:39]=[CH:38][C:34]([C:35]([N:52]5[CH2:57][CH2:56][O:55][CH2:54][CH2:53]5)=[O:36])=[CH:33][CH:32]=4)[CH:30]=3)[N:10]=2)[CH:5]=[C:6]([F:8])[CH:7]=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 4

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 682631,1'-CarbonyldiimidazoleHCID 67981025HCID 67981025、化合物

生成物 1

HCID 574072976-(3,5-difluorophenyl)-2-[(3-{1-[4-(morpholin-4-ylcarbonyl)phenyl]-1H-1,2,3-triazol-4-yl}-1H-indazol-5-yl)methyl]pyridazin-3(2H)-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
10 °C

実験手順

4-[4-(5-{[3-(3,5-difluorophenyl)-6-oxopyridazin-1(6H)-yl]methyl}-1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]benzoic acid (218 mg; 0.22 mmol; 1.0 eq.) was added in one portion to a suspension of 1,1′-carbonyldiimidazole (97 mg; 0.60 mmol; 2.7 eq.) in DMF (20 mL). The reaction suspension was heated at 10° C. for 20 min then morpholine (100 μl; 1.15 mmol; 5.2 eq.) was added in one portion. The reaction mixture was heated at 100° C. for 16 h. It was allowed to cool to RT, poured into HCl (1N solution) and extracted with EtOAc. Combined organic phases were washed sequentially with an aqueous saturated solution of NaHCO3 and brine, dried over magnesium sulfate, filtered and concentrated. The crude was purified by preparative HPLC to give the title compound a a white solid. 1H NMR (300 MHz, DMSO-d6) δ 13.42 (s, 1H), 9.38 (s, 1H), 8.48 (s, 1H), 8.23-8.08 (m, 3H), 7.75-7.64 (m, 4H), 7.61 (d, J=8.6 Hz, 1H), 7.57-7.48 (m, 1H), 7.42-7.28 (m, 1H), 7.13 (d, J=9.8 Hz, 1H), 5.51 (s, 2H), 3.64 (s, 8H). HPLC (Condition A): Rt 3.78 min (purity 97.7%). MS (ESI−): 593.7.

後処理

  1. temperatureThe reaction mixture was heated at 100° C. for 16 h
  2. temperatureto cool to RT
  3. extractionextracted with EtOAc
  4. washCombined organic phases were washed sequentially with an aqueous saturated solution of NaHCO3 and brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude was purified by preparative HPLC

出典と根拠

ORDレコード
ord-cf42100ac7bc4f3b970463d8d927f3bf
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073892B2

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