Hydrochloric Acid → HCID 67370777、化合物

HRID 1890763ノート

反応式

HRID 1890763 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:14]=[N:13][C:12]([N:15]3[CH2:20][CH2:19][CH:18]([N:21](C)[C:22](=O)OC(C)(C)C)[CH2:17][CH2:16]3)=[C:11]([CH3:30])[C:10]=2[CH3:31])=[CH:5][CH:4]=1)#[N:2].Cl>O1CCOCC1>[CH3:31][C:10]1[C:11]([CH3:30])=[C:12]([N:15]2[CH2:16][CH2:17][CH:18]([NH:21][CH3:22])[CH2:19][CH2:20]2)[N:13]=[N:14][C:9]=1[C:6]1[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58486412tert-Butyl 1-(6-(4-cyanophenyl)-4,5-dimethylpyridazin-3-yl)piperidin-4-yl(methyl)carbamate

生成物 1

HCID 67370777HCID 67370777、化合物収率 99.8%

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-cyanophenyl)-4,5-dimethylpyridazin-3-yl)piperidin-4-yl(methyl)carbamate (1.68 g, 3.99 mmol) in 1,4-dioxane (20 mL) with 4 M HCl in 1,4-dioxane (20 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, 20 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 a yellow solid (1.28 g, quantitative). ES/MS m/z 322.2 (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, 20 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-31e2bb2bf5fa40469978b1c6f83a497a
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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