Sulfuric Acid → HCID 919384, 화합물

HRID 1401416노트

반응식

HRID 1401416 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 919384HCID 919384, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bcc67513713f4d82940148ec987a0100
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907097B2

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