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4-Methoxybenzenesulfonyl chloride → HCID 247207, 화합물

HRID 1020461
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HRID 1020461 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](Cl)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 74014-Methoxybenzenesulfonyl chlorideHCID 31268Pyrrolidine

생성물 1

HCID 247207HCID 247207, 화합물수율 91.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

4-Methoxy-benzenesulfonyl chloride (3.00 g, 14.52 mmol) was slowly added to a solution of pyrrolidine (5.15 g, 72.6 mmol) in CHCl3 (15 mL) with stirring at 0° C. The reaction mixture was allowed to warm up to room temperature and then stirred for 1 hour. After that the reaction mixture was concentrated in vacuo. The residue was dissolved in toluene and washed with aqueous H3PO4 solution, and then aqueous KHCO3 solution. The organic phase was dried with Na2SO4, and filtered. The solvents were removed in vacuo and the residue crystallized from ether and heptane to provide the title compound (3.21 g, m.p. 88-89° C.).

후처리

  1. temperatureto warm up to room temperature
  2. stirringstirred for 1 hour
  3. concentrationAfter that the reaction mixture was concentrated in vacuo
  4. dissolutionThe residue was dissolved in toluene
  5. washwashed with aqueous H3PO4 solution
  6. dry with materialThe organic phase was dried with Na2SO4
  7. filtrationfiltered
  8. customThe solvents were removed in vacuo
  9. customthe residue crystallized from ether and heptane

출처 및 근거

ORD 기록
ord-7f0c53a315684873bed54c2a82112cb4
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716345B2

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