2-Aminobenzophenone → 2-(5-Oxotetrahydrofuran-2-carbonyl)aminobenzophenone

HRID 1774

반응식

HRID 1774 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[C:16](=[O:19])([O-])[OH:17].[Na+]>C(OCC)(=O)C>[O:19]=[C:16]1[O:17][CH:3]([C:4]([NH:1][C:2]2[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=2[C:4]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[O:5])=[O:5])[CH2:2][CH2:15]1

참가 물질

4

반응물 2

HCID 760802-AminobenzophenoneHCID 516892Sodium Bicarbonate

생성물 1

HCID 539323702-(5-Oxotetrahydrofuran-2-carbonyl)aminobenzophenone

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 4.9 g of 5-oxotetrahydrofuran-2-carboxylic acid and 5.5 ml of thionyl chloride was subjected to reflux for 2 hours. Thionyl chloride was then distilled off under reduced pressure to leave 5-oxotetrahydrofuran-2-carbonyl chloride. This product was mixed with 5.0 g of 2-aminobenzophenone, 200 ml of ethyl acetate and 200 ml of a saturated aqueous solution of sodium hydrogencarbonate, which was stirred for one hour at room temperature. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate, then the solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography (eluent, hexane:ethyl acetate=2:1) to give 2-(5-oxotetrahydrofuran-2-carbonyl)aminobenzophenone (6.5 g) as needles, m.p. 100° C.-102° C.

후처리

  1. washThe ethyl acetate layer was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by means of a silica gel column chromatography (eluent, hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-947d3e4afae94a0b8dd4f97535b58d90
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726306

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