Water → HCID 86625481, 화합물

HRID 2262963노트

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HRID 2262963 반응식
[N:1]1([C:7]2[O:11][C:10]([NH2:12])=[N:9][N:8]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.N1C=CC=CC=1.Cl[C:20]([O:22][CH2:23][C:24]([Cl:27])([Cl:26])[Cl:25])=[O:21].O>O1CCCC1>[N:1]1([C:7]2[O:11][C:10]([NH:12][C:20](=[O:21])[O:22][CH2:23][C:24]([Cl:27])([Cl:26])[Cl:25])=[N:9][N:8]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 870632,2,2-Trichloroethyl chloroformateHCID 27601385-Morpholin-4-yl-1,3,4-oxadiazol-2-ylamine

생성물 1

HCID 86625481HCID 86625481, 화합물수율 13.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-morpholin-4-yl-1,3,4-oxadiazol-2-ylamine (1.00 g, 5.88 mmol) and pyridine (0.570 ml, 7.05 mmol) in tetrahydrofuran (20 ml) was added, under ice-cooling, 2,2,2-trichloroethyl chloroformate (0.976 ml, 7.05 mmol), and the mixture was stirred at room temperature for 1 hour and half. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to yield 269 mg (13.3%) of the desired product as a solid.

후처리

  1. temperaturecooling
  2. extractionthe resulting solution was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-01915d7ee0014e5ebaa1c1b296ccd673
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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