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Dimethylformamide → HCID 57559893, 화합물

HRID 1724093
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HRID 1724093 반응식
[H-].[Na+].CN(C=O)C.[CH2:8]([O:11][C:12]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[CH:14][C:13]=1[SH:22])[CH2:9][CH3:10].Br[CH:24]1[CH2:29][CH2:28][N:27]([C:30]2[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][N:31]=2)[CH2:26][CH2:25]1>O>[CH2:8]([O:11][C:12]1[CH:17]=[C:16]([C:18]([F:19])([F:20])[F:21])[CH:15]=[CH:14][C:13]=1[S:22][CH:24]1[CH2:25][CH2:26][N:27]([C:30]2[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][N:31]=2)[CH2:28][CH2:29]1)[CH2:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 23159128HCID 23159128, 화합물HCID 23159146Pyridine, 2-(4-bromo-1-piperidinyl)-5-(trifluoromethyl)-

생성물 1

HCID 57559893HCID 57559893, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

After 60% sodium hydride was added, with chilling on ice, to the DMF (7 ml) solution of the chemical compound (46) (0.62 g), it was warmed to room temperature, and was then stirred for 30 minutes. After the chemical compound (48) (0.74 g) was added to the mixture, it was heated to 100° C., and was then stirred for 1 hour. After the mixture was cooled, it was poured into water, and was then subjected to extraction with ethyl acetate. After its organic layer was washed with water, and was then dried with anhydrous magnesium sulfate, it was filtered, and was then concentrated under reduced pressure. Its residue was purified by column chromatography to produce the chemical compound mentioned in the above title (0.90 g).

후처리

  1. temperaturewas heated to 100° C.
  2. stirringwas then stirred for 1 hour
  3. temperatureAfter the mixture was cooled
  4. extractionwas then subjected to extraction with ethyl acetate
  5. washAfter its organic layer was washed with water
  6. dry with materialwas then dried with anhydrous magnesium sulfate, it
  7. filtrationwas filtered
  8. concentrationwas then concentrated under reduced pressure
  9. customIts residue was purified by column chromatography
  10. customto produce the chemical compound

출처 및 근거

ORD 기록
ord-90f4e13ceb1343e9b2420ca4c67e06af
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07485727B2

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