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Phenacyl bromide → HCID 23143315, 화합물

HRID 732207
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HRID 732207 반응식
[CH2:1]([N:3]([CH2:11][CH3:12])[CH2:4][CH2:5][CH2:6][NH:7][C:8]([NH2:10])=[S:9])[CH3:2].Br[CH2:14][C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=O.[H-].[Na+].Cl[CH2:26][C:27]1[CH:46]=[CH:45][C:30]([CH2:31][O:32][C:33]2[CH:38]=[CH:37][C:36]([CH2:39][CH2:40][C:41]([O:43]C)=[O:42])=[CH:35][CH:34]=2)=[CH:29][CH:28]=1.P([O-])(O)(O)=O.[K+].[OH-].[Na+]>C(O)C.CN(C)C=O>[CH2:11]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][CH2:6][N:7]([CH2:26][C:27]1[CH:46]=[CH:45][C:30]([CH2:31][O:32][C:33]2[CH:38]=[CH:37][C:36]([CH2:39][CH2:40][C:41]([OH:43])=[O:42])=[CH:35][CH:34]=2)=[CH:29][CH:28]=1)[C:8]1[S:9][CH:14]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:10]=1)[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 6259Phenacyl bromideHCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 516951Monobasic potassium phosphate2회HCID 3034968Pseudourea, 3-(diethylaminopropyl)-2-thio-HCID 23082857Methyl 3-(4-([4-(chloromethyl)benzyl]oxy)phenyl)propanoate

생성물 1

HCID 23143315
HCID 23143315, 화합물
수율 53.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of N-[3-(diethylamino)propyl]thiourea (90 mg), 2-bromo-1-phenylethanone (100 mg) and N,N-dimethylformamide (3 mL) was stirred at room temperature for 1 hr. Sodium hydride (60% in oil, 40 mg) was added to the mixture under ice-cooling. The mixture was allowed to warm to room temperature and stirred for 1 hr. Methyl 3-(4-{[4-(chloromethyl)benzyl]-oxy}phenyl)propanoate (159 mg) was added to the reaction mixture under ice-cooling, allowed to warm to room temperature and stirred for 1 hr. The reaction mixture was poured into aqueous potassium dihydrogenphosphate solution and the mixture was extracted with ethyl acetate. The ethyl acetate layer was concentrated and the residue was purified by basic silica gel column chromatography to give a yellow oil. A mixture of the yellow oil, 2N aqueous sodium hydroxide solution (2 mL) and ethanol (5 mL) was stirred at room temperature for 1 hr. The reaction mixture was poured into aqueous potassium dihydrogenphosphate solution, and extracted with ethyl acetate. The ethyl acetate layer was dried using a Presep Dehydration tube (manufactured by Wako Pure Chemical Industries, Ltd.) and concentrated to give the title compound (142 mg, yield 51%) as a yellow oil.

후처리

  1. temperaturecooling
  2. temperatureto warm to room temperature
  3. stirringstirred for 1 hr
  4. temperaturecooling
  5. temperatureto warm to room temperature
  6. stirringstirred for 1 hr
  7. extractionthe mixture was extracted with ethyl acetate
  8. concentrationThe ethyl acetate layer was concentrated
  9. customthe residue was purified by basic silica gel column chromatography
  10. customto give a yellow oil
  11. stirringwas stirred at room temperature for 1 hr
  12. extractionextracted with ethyl acetate
  13. dry with materialThe ethyl acetate layer was dried
  14. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b2e362e7969f42948b9579cc03a9c2c8
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585880B2

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