Cyclopropylamine → 2-(Trimethylsilyl)ethyl 3-(cyclopropylsulfamoyl)benzoate

HRID 1025425

반응식

HRID 1025425 반응식
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:17]=[CH:18][CH:19]=1)[C:8]([O:10][CH2:11][CH2:12][Si:13]([CH3:16])([CH3:15])[CH3:14])=[O:9])(=[O:4])=[O:3].[CH:20]1([NH2:23])[CH2:22][CH2:21]1>N1C=CC=CC=1>[CH:20]1([NH:23][S:2]([C:5]2[CH:6]=[C:7]([CH:17]=[CH:18][CH:19]=2)[C:8]([O:10][CH2:11][CH2:12][Si:13]([CH3:16])([CH3:15])[CH3:14])=[O:9])(=[O:4])=[O:3])[CH2:22][CH2:21]1

참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 866763342-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate

생성물 1

HCID 712384462-(Trimethylsilyl)ethyl 3-(cyclopropylsulfamoyl)benzoate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2.00 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate, 1.2 mL of cyclopropylamine, and 20 mL of pyridine was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and to the residue was added an aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with 1.0 M hydrochloric acid and saturated brine in this order, then dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 2.12 g of 2-(trimethylsilyl)ethyl 3-(cyclopropylsulfamoyl)benzoate as a pale yellow oily substance. EI: 341

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionto the residue was added an aqueous citric acid solution
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe organic layer was washed with 1.0 M hydrochloric acid and saturated brine in this order
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ae01795146524e578c6a8793948035df
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729068B2

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