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Ethyl Acetate → HCID 59370741, 화합물

HRID 1873973
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HRID 1873973 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([O:11][Si](CC)(CC)CC)[CH2:9]I)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21].CCCC[N+](CCCC)(CCCC)CCCC.[F-].C1COCC1.C(OCC)(=O)C>C1COCC1.[Cl-].[Na+].O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:9][O:11]2)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 11078149TBAF tetrahydrofuranHCID 53922285HCID 53922285, 화합물

생성물 1

HCID 59370741HCID 59370741, 화합물수율 50%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 57417360Sodium chloride; water용매

실험 절차

(R)—N-(2-Chloro-5-(2-iodo-1-(triethylsilyloxy)ethyl)phenyl)methanesulfonamide (2.2308 g) was dissolved in dehydrated THF (40 mL), and added with 1 mol/L-TBAF-THF solution (10 mL; manufactured by Sigma-Aldrich Co.), followed by replacement with nitrogen and stirring at room temperature for 1 hour. The reaction solution was added to brine, and extraction was carried out once with ethyl acetate. The organic layer was washed once with water and dried over magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=71:29→50:50) to obtain the title compound (0.564 g).

후처리

  1. washThe organic layer was washed once with water
  2. dry with materialdried over magnesium sulfate
  3. customAfter the solvent was evaporated under reduced pressure
  4. customthe resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=71:29→50:50)

출처 및 근거

ORD 기록
ord-1efa9d0800c64757a83c6b6509cb88ce
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304443B2

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