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Chlorosulfonic acid → HCID 59180464, 화합물

HRID 1925740
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HRID 1925740 반응식
[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH2:11][CH2:10][CH2:9][CH2:8]1.Cl[S:14]([OH:17])(=[O:16])=[O:15]>ClCCl>[CH3:12][C:1]1[CH:6]=[C:5]([S:14]([OH:17])(=[O:16])=[O:15])[CH:4]=[CH:3][C:2]=1[N:7]1[CH2:11][CH2:10][CH2:9][CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 142531N-(2-Methylphenyl)pyrrolidine

생성물 1

HCID 59180464HCID 59180464, 화합물수율 96.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled (0° C.) solution of 119 (1.24 g; 7.7 mmol) in anhydrous dichloromethane (38 mL) was added chlorosulfonic acid (0.61 mL; 9.24 mmol) dropwise (1 mL/minutes). The reaction mixture w as allowed to gradually warm to room temperature while stirring overnight. The reaction mixture was concentrated under reduced pressure. The resulting oil w as taken up in diisopropyl ether (10 mL) and aqueous hydrochloric acid (0.5 mL; 2N) then stirred vigorously at room temperature for 2 hours. The organic phase was separated and concentrated under reduced pressure to yield the desired compound as an amber oil (1.8 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. stirringaqueous hydrochloric acid (0.5 mL; 2N) then stirred vigorously at room temperature for 2 hours
  3. customThe organic phase was separated
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2b8d1782863e4dd78ecd46edd2f54e78
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178699B2

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