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Sodium methanesulfinate → HCID 86697221, 화합물

HRID 237557
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HRID 237557 반응식
[CH3:1][S:2]([O-:4])=[O:3].[Na+].CS(O[CH2:11][C:12]([CH3:25])([CH3:24])[CH2:13][O:14][C:15]1[CH:20]=[C:19]([CH3:21])[C:18]([Br:22])=[C:17]([CH3:23])[CH:16]=1)(=O)=O>CN1CCCC1=O.C(OCC)C>[Br:22][C:18]1[C:17]([CH3:23])=[CH:16][C:15]([O:14][CH2:13][C:12]([CH3:25])([CH3:24])[CH2:11][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:20][C:19]=1[CH3:21]
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5

반응물 2

HCID 2733271Sodium methanesulfinateHCID 86697220HCID 86697220, 화합물

생성물 1

HCID 86697221HCID 86697221, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
180 °C

실험 절차

In a microwave vial sodium methanesulfinate (720 mg) is added to a solution of 3-(4-bromo-3,5-dimethylphenoxy)-2,2-dimethylpropyl methanesulfonate (271 mg) in N-methyl-2-pyrrolidinon (NMP) (8 mL). The mixture is heated to 180° C. for 30 minutes. Then the mixture is diluted with diethylether, washed with water and brine and dried (MgSO4). The solvent is evaporated and the residue is purified by HPLC on reversed phase to give the title compound. Yield: 32 mg; LC (method 8): tR=0.47 min; Mass spectrum (ESI+): m/z=349 [M+H]+.

후처리

  1. washwashed with water and brine
  2. dry with materialdried (MgSO4)
  3. customThe solvent is evaporated
  4. customthe residue is purified by HPLC on reversed phase

출처 및 근거

ORD 기록
ord-98a6589c2afd422288c2787a5234b7d5
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642585B2

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