Tert-Butylamine → ethyl-2-(N-tert-butylsulfamoyl)acetate

HRID 553464

반응식

HRID 553464 반응식
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[CH2:6]([O:8][C:9]([CH2:11][S:12](Cl)(=[O:14])=[O:13])=[O:10])[CH3:7]>C1COCC1>[CH2:6]([O:8][C:9](=[O:10])[CH2:11][S:12](=[O:14])(=[O:13])[NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH3:7]

참가 물질

4

반응물 2

HCID 6385Tert-ButylamineHCID 12225100Ethyl (chlorosulfonyl)acetate

생성물 1

HCID 19833529ethyl-2-(N-tert-butylsulfamoyl)acetate수율 43%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-20 °C

실험 절차

tert-Butylamine (7.9 mL, 75 mmol.) was dissolved in 50 mL of THF. The solution was cooled to −20° C. and (ethoxycarbonyl)methanesulfonyl chloride dissolved in 10 mL of THF was added slowly. The reaction mixture was allowed to warm to room temperature and stirred for 24 h. The mixture was filtered, and the filtrate concentrated in vacuo. The residue was purified by column chromatography (PE/EtOAc; 2:1) to afford ethyl-2-(N-tert-butylsulfamoyl)acetate (4.1 g, 43%).

후처리

  1. additionwas added slowly
  2. temperatureto warm to room temperature
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate concentrated in vacuo
  5. customThe residue was purified by column chromatography (PE/EtOAc; 2:1)

출처 및 근거

ORD 기록
ord-794c0450771447b48a4f95417416d507
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048862B2

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