Triethylamine → HCID 70211079, 화합물

HRID 1068728노트

반응식

HRID 1068728 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[C:13]2[N:8]3[C:9](=[N:14][C:15]([CH3:16])=[C:7]3[C:6]1=[O:17])[CH:10]=[CH:11][CH:12]=2.C(N(CC)CC)C.[F:25][C:26]([F:33])([F:32])[CH2:27][S:28](Cl)(=[O:30])=[O:29]>C(Cl)Cl>[CH3:16][C:15]1[N:14]=[C:9]2[CH:10]=[CH:11][CH:12]=[C:13]3[N:8]2[C:7]=1[C:6](=[O:17])[N:5]3[CH2:4][CH2:3][CH2:2][NH:1][S:28]([CH2:27][C:26]([F:33])([F:32])[F:25])(=[O:30])=[O:29]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 742422,2,2-Trifluoroethanesulfonyl chlorideHCID 211900961-[3-(Amino)propan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one

생성물 1

HCID 70211079HCID 70211079, 화합물수율 58.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.43 g (1.87 mmol) of 1-[3-(amino)propan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one and 0.39 ml (2.80 mmol) of triethylamine in 30 ml of methylene chloride was added, while stirring under ice-cooling, 0.41 g (2.26 mmol) of 2,2,2-trifluoroethanesulfonyl chloride. The mixture was stirred for 30 minutes at the same temperature. The reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which was then dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate) to give 412 mg of the desired compound (58.6%, white powdery).

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred for 30 minutes at the same temperature
  3. washThe reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which
  4. dry with materialwas then dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was purified by column chromatography (eluent: ethyl acetate)

출처 및 근거

ORD 기록
ord-dd3d1a19e4c44fe7b26332c23afe8d7c
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251905B1

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