Hydrochloric Acid → 1-Phenylpyrazol-5-ylamine

HRID 1260469

反応式

HRID 1260469 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1C(OCC)=O.Cl.[NH4+].[OH-]>>[C:7]1([N:6]2[C:2]([NH2:1])=[CH:3][CH:4]=[N:5]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 85270Ethyl 5-amino-1-phenyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 700061-Phenylpyrazol-5-ylamine収率 94%

実験手順

5-Amino-4-carbethoxy-1-phenylpyrazole (1 eq.) was dissolved in 36% HCl solution (30 eq.) and the reaction mixture was stirred under reflux for overnight. The mixture was cooled, poured onto ice and made basic with NH4OH. The mixture was extracted with DCM (×3). The combined organic fractions were washed with brine, dried (Na2SO4), and the solvent was evaporated under reduced pressure to obtain the product as pale yellow oil in 94% yield. MS (ES+) C9H9N3 requires 159, found: 160 (M+H)+.

後処理

  1. temperatureunder reflux for overnight
  2. temperatureThe mixture was cooled
  3. additionpoured onto ice
  4. extractionThe mixture was extracted with DCM (×3)
  5. washThe combined organic fractions were washed with brine
  6. dry with materialdried (Na2SO4)
  7. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-e2f183bfde9840139d413b9b940b96d3
出典データセット
uspto-grants-2013_06
特許番号
US08470823B2

関連ノート

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