Hydrochloric Acid → 1-(4-methanesulfonyl-phenyl)-1H-pyrazole

HRID 2060080

反応式

HRID 2060080 の反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][NH2:12])=[CH:7][CH:6]=1)(=[O:4])=[O:3].CO[CH:15](OC)[CH2:16][CH:17](OC)OC.Cl>C(O)C>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH:17]=[CH:16][CH:15]=[N:12]2)=[CH:9][CH:10]=1)(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 66019TetramethoxypropaneHCID 701424-(Methylsulphonyl)phenylhydrazine

生成物 1

HCID 214780151-(4-methanesulfonyl-phenyl)-1H-pyrazole収率 79%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

To a solution of 4-(methylsulfonyl)phenylhydrazine (5.0 g, 26.8 mmol, 1.00 equiv) and 1,1,3,3-tetramethoxypropane (4.4 mL, 26.8, 1.0 equiv) in ethanol (37 mL) at rt was added concentrated HCl (2.8 mL). The resulting solution was heated at reflux for 1 hr, cooled to 0° C. and filtered to give 1-(4-methanesulfonyl-phenyl)-1H-pyrazole as a yellow solid (4.73 g, 79%). LCMS: (MH)+=223.1 (1.19 min).

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux for 1 hr
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-cf5f16db644e423890a415b90ce6cc83
出典データセット
uspto-grants-2012_10
特許番号
US08278337B2

関連ノート

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