Tetrahydrofuran → 2-Methyl-N-(oxetan-3-ylidene)propane-2-sulfinamide

HRID 624272

반응식

HRID 624272 반응식
[CH3:1][C:2]([S:5]([NH2:7])=[O:6])([CH3:4])[CH3:3].[O:8]1[CH2:12][CH2:11][CH2:10]C1.O1CC(=O)C1>[Cl-].[Na+].O.C(O[Ti](OCC)(OCC)OCC)C>[CH3:1][C:2]([S:5]([N:7]=[C:11]1[CH2:10][O:8][CH2:12]1)=[O:6])([CH3:4])[CH3:3]

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 3382465Tert-ButanesulfinamideHCID 150242543-Oxetanone

생성물 1

HCID 468399952-Methyl-N-(oxetan-3-ylidene)propane-2-sulfinamide

시약·촉매·용매 2

HCID 178477244HCID 178477244, 화합물촉매HCID 57417360Sodium chloride; water용매

반응 조건

온도
50 °C

실험 절차

To a 250 mL round-bottomed flask was added 2-methylpropane-2-sulfinamide (3.36 g, 27.8 mmol) followed by tetraethoxytitanium (11.64 ml, 55.5 mmol) to a tetrahydrofuran (69.4 ml) solution of oxetan-3-one (2 g, 27.8 mmol) at room temperature. The mixture was stirred at 50° C. for 5 hours, cooled and poured into brine. The suspension was filtered through a pad of diatomaceous earth eluting with ethyl acetate. The organics were combined, dried with sodium sulfate, filtered and concentrated under vacuum. The residue was purified by regular phase flash column chromatography to give the title compound.

후처리

  1. temperaturecooled
  2. filtrationThe suspension was filtered through a pad of diatomaceous earth
  3. washeluting with ethyl acetate
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customThe residue was purified by regular phase flash column chromatography

출처 및 근거

ORD 기록
ord-3d453ee755554741a9d6bc4cb6c12527
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302989B2

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