Hydrochloric Acid → HCID 67368812、化合物

HRID 1890762ノート

反応式

HRID 1890762 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([N:14]3[CH2:19][CH2:18][CH:17]([N:20](C)[C:21](=O)OC(C)(C)C)[CH2:16][CH2:15]3)=[C:10]([CH3:29])[C:9]=2[CH3:30])=[CH:4][CH:3]=1.Cl>O1CCOCC1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[N:12][C:11]([N:14]3[CH2:19][CH2:18][CH:17]([NH:20][CH3:21])[CH2:16][CH2:15]3)=[C:10]([CH3:29])[C:9]=2[CH3:30])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58486414HCID 58486414、化合物

生成物 1

HCID 67368812HCID 67368812、化合物収率 99.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

Treat a solution of tert-butyl 1-(6-(4-fluorophenyl)-4,5-dimethylpyridazin-3-yl)piperidin-4-yl(methyl)carbamate (1.04 g, 2.51 mmol) in 1,4-dioxane (10 mL) with 4 M HCl in 1,4-dioxane (15.0 mL). Stir the resulting mixture at ambient temperature for 2 h. Concentrate the reaction mixture under reduced pressure. Dissolve the residue in MeOH, and pour onto an SCX column (Varian, 10 g). Rinse the column with MeOH and CH2Cl2, and elute the product with a 1:1 mixture of CH2Cl2 and 2 M NH3/MeOH. Concentrate under reduced pressure to afford the title compound as an off-white solid (784 mg, 99%). ES/MS m/z 315.2 (M+1).

後処理

  1. concentrationConcentrate the reaction mixture under reduced pressure
  2. dissolutionDissolve the residue in MeOH
  3. additionpour onto an SCX column (Varian, 10 g)
  4. washRinse the column with MeOH and CH2Cl2
  5. washelute the product
  6. additionwith a 1:1 mixture of CH2Cl2 and 2 M NH3/MeOH
  7. concentrationConcentrate under reduced pressure

出典と根拠

ORDレコード
ord-30303adb12984eeaa089d9231cab2b76
出典データセット
uspto-grants-2013_08
特許番号
US08507490B2

反応ノート

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