Dimethylformamide → 6-(3-Phenylpropoxy)-2-(2-pyridyl)-4H-1,3-benzothiazine-4-one

HRID 499364노트

반응식

HRID 499364 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=3)=[N:8][C:7](=[O:17])[C:6]=2[CH:18]=1.Br[CH2:20][CH2:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>O>[C:23]1([CH2:22][CH2:21][CH2:20][O:1][C:2]2[CH:3]=[CH:4][C:5]3[S:10][C:9]([C:11]4[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=4)=[N:8][C:7](=[O:17])[C:6]=3[CH:18]=2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 12503(3-Bromopropyl)benzeneHCID 229394706-hydroxy-2-(2-pyridyl)-4H-1,3-benzothiazine-4-one

생성물 1

HCID 597501196-(3-Phenylpropoxy)-2-(2-pyridyl)-4H-1,3-benzothiazine-4-one수율 98.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 6-hydroxy-2-(2-pyridyl)-4H-1,3-benzothiazine-4-one (0.35 g, 1.3 mmol), 1-bromo-3-phenylpropane (0.86 g, 4.3 mmol) and potassium carbonate (0.38 g, 2.7 mmol) and DMF (10 ml) was stirred at room temperature for 20 hrs. The reaction mixture was diluted with water and extracted with ethyl acetate. The extract was washed with water and dried. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from tetrahydrofuran-hexane to give the titled compound (0.48 g, 92%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customThe solvent was evaporated under reduced pressure
  5. customThe obtained crystals were recrystallized from tetrahydrofuran-hexane

출처 및 근거

ORD 기록
ord-580202ea30da44498bb684e0116059a2
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767665B2

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