Trifluoroacetic acid → HCID 59075091, 화합물

HRID 2184337노트

반응식

HRID 2184337 반응식
[OH:1][CH2:2][C@@H:3]1[NH:7][C:6](=[O:8])[C:5]([CH3:10])([CH3:9])[CH2:4]1.[CH:11]([O:13][CH2:14][CH3:15])=[CH2:12].FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[CH2:11]([O:13][CH:14]([O:1][CH2:2][C@@H:3]1[NH:7][C:6](=[O:8])[C:5]([CH3:10])([CH3:9])[CH2:4]1)[CH3:15])[CH3:12]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 8023Ethyl vinyl etherHCID 59075103HCID 59075103, 화합물

생성물 1

HCID 59075091HCID 59075091, 화합물수율 43.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of (R)-5-hydroxymethyl-3,3-dimethyl-pyrrolidin-2-one (4.0 g, 28 mmol), prepared as described in Tetrahedron 1998, 54 10295-10307, and ethyl vinyl ether (4 mL, 42 mmol) in chloroform (26 mL), was added a catalytic amount of trifluoroacetic acid (0.056 mL), and the reaction mixture was stirred for four hours at room temperature. The solution was then washed with a saturated solution of sodium bicarbonate and brine, and dried over magnesium sulfate. The crude oil obtained after evaporating the solvent, was purified by chromatography on silica gel using hexane:ethyl acetate 1:1 as a solvent, giving 2.6 g of (R)-5-(1-ethoxy-ethoxymethyl)-3,3-dimethyl-pyrrolidin-2-one.

후처리

  1. washThe solution was then washed with a saturated solution of sodium bicarbonate and brine
  2. dry with materialdried over magnesium sulfate
  3. customThe crude oil obtained
  4. customafter evaporating the solvent
  5. customwas purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-9915ae513afa47158494a076450f7fa0
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900336B2

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