2,4-Hexadienoyl chloride → HCID 86589101, 화합물

HRID 1268137

반응식

HRID 1268137 반응식
[C:1](Cl)(=[O:7])[CH:2]=[CH:3][CH:4]=[CH:5][CH3:6].[C:9]1([C:15]#[C:16][C:17]2[CH:35]=[CH:34][C:20]([C:21]([NH:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[S:30](=[O:33])(=[O:32])[NH2:31])=[O:22])=[CH:19][CH:18]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CN(C)C1C=CN=CC=1.O1CCCC1>[C:9]1([C:15]#[C:16][C:17]2[CH:35]=[CH:34][C:20]([C:21]([NH:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[S:30]([NH:31][C:1](=[O:7])/[CH:2]=[CH:3]/[CH:4]=[CH:5][CH3:6])(=[O:33])=[O:32])=[O:22])=[CH:19][CH:18]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

5

반응물 2

HCID 5653802,4-Hexadienoyl chlorideHCID 120430434-Phenylethynyl-N-(2-sulfamoylphenyl)benzamide

생성물 1

HCID 86589101HCID 86589101, 화합물수율 48%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매

실험 절차

In a stream of nitrogen and at 0° C., 0.10 ml (0.96 mmol) of 2,4-hexadienoyl chloride was added to an anhydrous tetrahydrofuran (10 ml) solution containing 300 mg (0.80 mmol) of 4-phenylethynyl-N-(2-sulfamoylphenyl)benzamide produced in Reference Example 10 and 195 mg (1.60 mmol) of 4-dimethylaminopyridine, the mixture was stirred at room temperature for 1 hour and then the solvent was evaporated under a reduced pressure. The resulting residue was dissolved in ethyl acetate, washed with water, a potassium hydrgensulfate aqueous solution and saturated brine in that order and dried over anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The thus formed crude crystals were recrystallized from methanol to obtain 180 mg (yield: 48.0%) of the title compound.

후처리

  1. customthe solvent was evaporated under a reduced pressure
  2. dissolutionThe resulting residue was dissolved in ethyl acetate
  3. washwashed with water
  4. dry with materiala potassium hydrgensulfate aqueous solution and saturated brine in that order and dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under a reduced pressure
  6. customThe thus formed crude crystals
  7. customwere recrystallized from methanol

출처 및 근거

ORD 기록
ord-b2d1a8e90dff406aa95a2c9993fc90b3
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06555584B1

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