Water → HCID 59310058, 화합물

HRID 1512987노트

반응식

HRID 1512987 반응식
[Cl:1][C:2]1[C:7]([N:8]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]2=[O:18])=[CH:6][C:5]([S:19](Cl)(=O)=O)=[C:4]([O:23][CH3:24])[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O.C(OCC)(=O)C>O1CCCC1>[Cl:1][C:2]1[C:7]([N:8]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]2=[O:18])=[CH:6][C:5]([SH:19])=[C:4]([O:23][CH3:24])[CH:3]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 8857Ethyl AcetateHCID 11776TriphenylphosphineHCID 59310094HCID 59310094, 화합물

생성물 1

HCID 59310058HCID 59310058, 화합물수율 90.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 4-chloro-5-(1,3-dioxo-1,3-dihydroisoindol-2-yl)-2-methoxy-benzenesulfonyl chloride (0.83 g) in tetrahydrofuran (10 mL) were added triphenylphosphine (1.98 g) and water (1.5 mL), and the mixture was stirred at room temperature overnight. To the reaction mixture were added water and ethyl acetate, and the organic layer was separated. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1) to give the title compound (0.62 g).

후처리

  1. customthe organic layer was separated
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-6f524bde285a40aeaff4afd743b5017c
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217069B2

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