Water → HCID 68777852, 화합물

HRID 2263022노트

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HRID 2263022 반응식
Cl[C:2]1[S:6][N:5]=[C:4]([C:7]2[S:8][CH:9]=[CH:10][CH:11]=2)[N:3]=1.[N:12]1([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(N(CC)CC)C.O>CN(C)C=O>[S:8]1[CH:9]=[CH:10][CH:11]=[C:7]1[C:4]1[N:3]=[C:2]([N:15]2[CH2:14][CH2:13][N:12]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16]2)[S:6][N:5]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 27358235-Chloro-3-(2-thienyl)-1,2,4-thiadiazole

생성물 1

HCID 68777852HCID 68777852, 화합물수율 51.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-chloro-3-(2-thienyl)-1,2,4-thiadiazole (4.80 g, 23.7 mmol) and tert-butyl piperazine-1-carboxylate (4.41 g, 23.7 mmol) in dimethylformamide (50 ml) was added triethylamine (13.2 ml, 94.7 mmol) at room temperature, and the mixture was stirred at room temperature for 1 hour. 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 recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 4.33 g (51.9%) of the desired product as a solid.

후처리

  1. extractionthe resulting solution was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was recrystallized from a mixed solvent of hexane and tetrahydrofuran

출처 및 근거

ORD 기록
ord-09651ac4969b493181448efc97fae428
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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