Cesium carbonate → HCID 69231272, 화합물

HRID 30396

반응식

HRID 30396 반응식
[CH3:1][S:2]([CH2:5][C:6]([O:8][CH3:9])=[O:7])(=[O:4])=[O:3].I[CH2:11][CH2:12][CH2:13]I.C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C>[CH3:1][S:2]([C:5]1([C:6]([O:8][CH3:9])=[O:7])[CH2:13][CH2:12][CH2:11]1)(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 123141,3-DiiodopropaneHCID 2759918Methanesulfonylacetic acid methyl ester

생성물 1

HCID 69231272HCID 69231272, 화합물수율 79%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of methyl methylsulfonylacetate (1.0 g, 6.6 mmol) in 20 mL of acetonitrile was added 1,3-diiodopropane (2.3 mL, 20 mmol) and cesium carbonate (6.4 g, 20 mmol). After stirring at room temperature for 2 h, the reaction was partitioned between water (50 mL) and ethyl acetate (100 mL). The organic layer was separated, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness, and the residue was purified by flash chromatography on silica gel eluting with 20 to 50% ethyl acetate in hexane to give methyl 1-methylsulfonylcyclobutanecarboxlate (1.0 g, 79%). δ 3.84 (s, 3H), 3.02 (s, 3H), 2.84-2.65 (m, 4H), 2.25-2.02 (m, 2H).

후처리

  1. customthe reaction was partitioned between water (50 mL) and ethyl acetate (100 mL)
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customthe residue was purified by flash chromatography on silica gel eluting with 20 to 50% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-c4ab329b32dc4ec78c61c1605479c0ea
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423067B2

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