Water → HCID 86625481、化合物

HRID 2262963ノート

反応式

HRID 2262963 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 86625481HCID 86625481、化合物収率 13.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-01915d7ee0014e5ebaa1c1b296ccd673
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

反応ノート

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