Water → HCID 68778698, 화합물

HRID 2263240노트

반응식

HRID 2263240 반응식
C(N(CC)CC)C.[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)=[O:14])([CH3:11])([CH3:10])[CH3:9].Cl[C:22]1[S:26][N:25]=[C:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[F:33])[N:23]=1.O>CN(C)C=O>[F:33][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=1[C:24]1[N:23]=[C:22]([N:18]2[CH2:19][CH2:20][N:15]([C:13]([O:12][C:8]([CH3:11])([CH3:9])[CH3:10])=[O:14])[CH2:16][CH2:17]2)[S:26][N:25]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 463184775-Chloro-3-(2-fluorophenyl)-1,2,4-thiadiazole

생성물 1

HCID 68778698HCID 68778698, 화합물수율 65.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Triethylamine (14.7 ml, 105 mmol) was added to a solution of 1-(tert-butoxycarbonyl)piperazine (5.64 g, 26.3 mmol) and 5-chloro-3-(2-fluorophenyl)-1,2,4-thiadiazole (4.89 g, 26.3 mmol) in N,N-dimethylformamide (100 ml), the mixture was stirred was stirred at room temperature for 30 minutes, the reaction mixture was poured into water, and the mixture 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 ethyl acetate to give 6.28 g (65.6%) of the desired product as a crystal.

후처리

  1. stirringwas stirred at room temperature for 30 minutes
  2. extractionthe mixture 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 recrystallized from a mixed solvent of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-fbaff1440ecc4eacbf73afa094298b4c
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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