Hydrochloric Acid → 1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride

HRID 1770544

反応式

HRID 1770544 の反応式
[CH3:1][C:2]1[C:6]([CH2:7][N:8]2[CH:12]=[C:11]([NH:13]C(=O)OC(C)(C)C)[CH:10]=[N:9]2)=[C:5]([CH3:21])[O:4][N:3]=1.[ClH:22]>O1CCOCC1>[ClH:22].[CH3:1][C:2]1[C:6]([CH2:7][N:8]2[CH:12]=[C:11]([NH2:13])[CH:10]=[N:9]2)=[C:5]([CH3:21])[O:4][N:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57945015Tert-butyl 1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-ylcarbamate

生成物 1

HCID 574222641-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride収率 99%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Tert-butyl 1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-ylcarbamate (example 10-41b) (592 mg, 2 mmol) was stirred in a solution of 4N HCl in dioxane (20 mL) at ambient temperature for 2 hours. The solvent was removed and the residue was dissolved in a 1/1 mixture of ethyl acetate/hexanes (30 mL) and concentrated twice. The solid was triturated with hexanes and collected by filtration providing 1-((3,5-dimethylisoxazol-4-yl)methyl)-1H-pyrazol-4-amine hydrochloride (500 mg, 99%) as a white solid. 1H NMR (DMSO-d6, 400 MHz); δ 2.11 (s, 3H), 2.38 (s, 3H), 5.16 (s, 2H), 7.51 (s, 1H), 8.03 (s, 1H), 10.27 (bs, 3H).

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in a 1/1 mixture of ethyl acetate/hexanes (30 mL)
  3. concentrationconcentrated twice
  4. customThe solid was triturated with hexanes
  5. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-b0c9a716ec78477ab39c0d2e5de6beda
出典データセット
uspto-grants-2016_02
特許番号
US09247759B2

関連ノート

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