Hydrochloric Acid → HCID 67370777, 화합물

HRID 1890763노트

반응식

HRID 1890763 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 67370777HCID 67370777, 화합물수율 99.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-31e2bb2bf5fa40469978b1c6f83a497a
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507490B2

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