Water → HCID 59310058、化合物

HRID 1512987ノート

反応式

HRID 1512987 の反応式
[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

参加物

6

反応物 4

HCID 962Water2 回HCID 8857Ethyl AcetateHCID 11776TriphenylphosphineHCID 59310094HCID 59310094、化合物

生成物 1

HCID 59310058HCID 59310058、化合物収率 90.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6f524bde285a40aeaff4afd743b5017c
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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