Hydrochloric Acid → 1227070-38-3

HRID 1890772ノート

反応式

HRID 1890772 の反応式
[Li+].[OH-].[CH3:3][N:4]1[C:8]([S:9]([CH3:12])(=[O:11])=[O:10])=[C:7]([C:13]([O:15]CC)=[O:14])[CH:6]=[N:5]1.Cl>O.O1CCOCC1>[CH3:3][N:4]1[C:8]([S:9]([CH3:12])(=[O:10])=[O:11])=[C:7]([C:13]([OH:15])=[O:14])[CH:6]=[N:5]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2 回HCID 58486417Ethyl 1-methyl-5-(methylsulfonyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 584864151227070-38-3収率 64%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

Add a solution of LiOH (22 mg, 0.90 mmol) in H2O (1 mL) to a rapidly stirring solution of ethyl 1-methyl-5-(methylsulfonyl)-1H-pyrazole-4-carboxylate (175 mg, 0.75 mmol) in 1,4-dioxane (3 mL) at ambient temperature. Treat the reaction mixture with additional LiOH (5 mg, 0.21 mmol), and stir overnight. Acidify to pH 2 with 1 N HCl, and extract twice with CH2Cl2. Combine the organic layers, dry over MgSO4, filter, and concentrate under reduced pressure to yield the title compound as a white solid (98 mg, 64%). ES/MS m/z 202.9 (M−1).

後処理

  1. extractionextract twice with CH2Cl2
  2. dry with materialdry over MgSO4
  3. filtrationfilter
  4. concentrationconcentrate under reduced pressure

出典と根拠

ORDレコード
ord-efc60d9c63f544b1b55dbe8200460ea7
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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