Sulfuric Acid → HCID 919384、化合物

HRID 1400340ノート

反応式

HRID 1400340 の反応式
S(=O)(=O)(O)O.Cl.[F:7][C:8]1[CH:13]=[CH:12][C:11]([NH:14]N)=[CH:10][CH:9]=1.[CH3:16][N:17]1[CH2:22][CH2:21][CH2:20][CH2:19][C:18]1=O>O1CCOCC1>[F:7][C:8]1[CH:13]=[CH:12][C:11]2[NH:14][C:20]3[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][C:19]=3[C:10]=2[CH:9]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 13603N-Methyl-2-piperidoneHCID 699814-Fluorophenylhydrazine hydrochloride

生成物 1

HCID 919384HCID 919384、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Sulfuric acid is added to a solution of 4-fluorophenyl hydrazine hydrochloride (1 equiv.) in dioxane and stirred for 5 min. at RT. N-Methyl piperidone (0.76-1.4 equiv.) is added and the mixture is heated at 80° C. for 2 h. After completion, as monitored by TLC, the reaction mixture is concentrated under reduced pressure and basified to pH 10 using 10% aqueous KOH solution. The reaction mixture is extracted with EtOAc, dried over anhydrous sodium sulfate and concentrated under reduced pressure using rotary evaporator to provide the desired compound.

後処理

  1. temperaturethe mixture is heated at 80° C. for 2 h
  2. concentrationthe reaction mixture is concentrated under reduced pressure and basified to pH 10
  3. extractionThe reaction mixture is extracted with EtOAc
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customevaporator

出典と根拠

ORDレコード
ord-190a521c04f646f1b57c69cfe270dc1d
出典データセット
uspto-grants-2014_12
特許番号
US08906925B2

反応ノート

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