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2-Bromo-N-methyl-N-phenylacetamide → HCID 14855467, 화합물

HRID 477391
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HRID 477391 반응식
[Na].[F:2][C:3]([F:14])([C:8]1[CH:12]=[C:11]([OH:13])[O:10][N:9]=1)[C:4]([F:7])([F:6])[F:5].[CH3:15][N:16]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:17](=[O:20])[CH2:18]Br>C(#N)C>[CH3:15][N:16]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:17](=[O:20])[CH2:18][O:13][C:11]1[O:10][N:9]=[C:8]([C:3]([F:2])([F:14])[C:4]([F:7])([F:6])[F:5])[CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 344952-Bromo-N-methyl-N-phenylacetamideHCID 178516125HCID 178516125, 화합물

생성물 1

HCID 14855467HCID 14855467, 화합물수율 67.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

To 0.50 g (2.2 mmole) of 3-pentafluoroethyl-5-hydroxyisoxazole sodium salt were added dry acetonitrile (7 ml) and N-methyl-N-phenyl-2-bromoacetamide (0.55 g) and the resulting mixture was stirred at 60° C. for 24 hours. After completion of reaction, the reaction solution was evaporated under reduced pressure and to the residue was added water (80 ml), extracted with methylene chloride, treated with anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by chromatography on silica gel to give 0.52 g of crystals. These crystals were recrystallized from n-hexane to give 0.48 g of the titled compound as colorless plates, yield 62.3%, m.p. 88.0-89.0° C.

후처리

  1. customAfter completion of reaction
  2. customthe reaction solution was evaporated under reduced pressure and to the residue
  3. additionwas added water (80 ml)
  4. extractionextracted with methylene chloride
  5. additiontreated with anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-ebc78d76f1ca42829655549d9ef96307
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04888044

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