Water → HCID 11573382, 화합물

HRID 1282141노트

반응식

HRID 1282141 반응식
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=1.[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[N:20]1[CH2:21][CH2:22][N:23]([CH2:2][C:3]2[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=2)[CH2:24][CH2:25]1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 944591-(2-Pyridyl)piperazineHCID 15550682N-((4-(chloromethyl)phenyl)methyl)acetamide

생성물 1

HCID 11573382HCID 11573382, 화합물수율 152.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of N-(4-chloromethylphenylmethyl)acetamide (1.0 g), 1-(2-pyridyl)piperazine (1.4 g) and potassium carbonate (4.2 g) in dimethylformamide (20 ml) was stirred at 60-70° C. for 2.5 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a brown oil. The obtained brown oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=20:1) to give a pale-yellow oil (2.5 g). The obtained pale-yellow oil was crystallized from ethyl acetate and the crystals were recrystallized from ethyl acetate to give the title compound (1.4 g) as white crystals, m.p.=100-101° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customto give a brown oil
  6. customThe obtained brown oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=20:1)

출처 및 근거

ORD 기록
ord-98984b14b4c54139ac09bc93bdd7cf85
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455528B1

반응 노트

불러오는 중…