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Hydrochloric Acid → (Rac)-2-(4-{3-[1-(3-methyl-3h-benzoimidazol-5-yl)-ethyl]-imidazo[1,2-b]pyridazin-6-yl}-pyrazol-1-yl)-ethanol

HRID 69228
ノート
印刷プレビュー

反応式

HRID 69228 の反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([CH:11]([C:13]3[N:17]4[N:18]=[C:19]([C:22]5[CH:23]=[N:24][N:25]([CH2:27][CH2:28][O:29]C6CCCCO6)[CH:26]=5)[CH:20]=[CH:21][C:16]4=[N:15][CH:14]=3)[CH3:12])[CH:9]=[CH:10][C:5]=2[N:4]=[CH:3]1.Cl>C(Cl)Cl.CO.O1CCOCC1>[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([CH:11]([C:13]3[N:17]4[N:18]=[C:19]([C:22]5[CH:23]=[N:24][N:25]([CH2:27][CH2:28][OH:29])[CH:26]=5)[CH:20]=[CH:21][C:16]4=[N:15][CH:14]=3)[CH3:12])[CH:9]=[CH:10][C:5]=2[N:4]=[CH:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 68633396(Rac)-3-[1-(3-methyl-3h-benzoimidazol-5-yl)-ethyl]-6-{1-[2-(tetrahydro-pyran-2-yloxy)-ethyl]-1h-pyrazol-4-yl}-imidazo[1,2-b]pyridazine

生成物 1

HCID 57917436(Rac)-2-(4-{3-[1-(3-methyl-3h-benzoimidazol-5-yl)-ethyl]-imidazo[1,2-b]pyridazin-6-yl}-pyrazol-1-yl)-ethanol

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6344
Dichloromethane
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

(rac)-3-[1-(3-Methyl-3H-benzoimidazol-5-yl)-ethyl]-6-{1-[2-(tetrahydro-pyran-2-yloxy)-ethyl]-1H-pyrazol-4-yl}-imidazo[1,2-b]pyridazine (Stage 185.1, 600 mg, 1.018 mmol) was dissolved in DCM (10 mL) and MeOH (2.5 mL). HCl in dioxane (4 N, 1.272 mL) was added and the RM was stirred 1 h at rt. The solvent was totally evaporated and the residue taken in water /acetonitrile. It was basified with NaHCO3. the mixture was cooled down with dry ice and sonicated to afford a suspension. It was filtered and collected, and dried under high vacuum overnight to afford the title compound as a white solid (tR 2.04 min (conditions 8), MH+=388, 1H-NMR in DMSO-d6: 8.39 (s, 1H); 8.07 (d, 2H); 8.01 (d, 1H); 7.69 (s, 1H); 7.61 (s, 1H); 7.51 (d, 1H); 7.47 (d, 1H); 7.23 (d, 1H); 4.95 (t, 1H); 4.76 (q, 1H); 4.18 (t, 2H); 3.78 (s, 3H); 3.75 (q, 2H); 1.79 (d, 3H)).

後処理

  1. customThe solvent was totally evaporated
  2. temperaturethe mixture was cooled down with dry ice
  3. customsonicated
  4. customto afford a suspension
  5. filtrationIt was filtered
  6. customcollected
  7. customdried under high vacuum overnight

出典と根拠

ORDレコード
ord-4968c7be8dac4a4bb928fde6ecf62a9b
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822468B2

反応ノート

読み込み中…

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