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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sulfuric Acid → HCID 21588280, 화합물

HRID 463444
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HRID 463444 반응식
[CH3:1][NH:2][C:3](=[O:12])[CH:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[OH:5].S(=O)(=O)(O)O.C(Cl)(Cl)Cl.[CH:22]1[CH:27]=CC=CC=1.C[OH:29]>C(OC(=O)C)(=O)C>[CH3:1][NH:2][C:3](=[O:12])[CH:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[O:5][C:27](=[O:29])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 6212ChloroformHCID 5720632-hydroxy-N-methyl-2-phenylacetamideHCID 21927730Benzene methanol

생성물 1

HCID 21588280HCID 21588280, 화합물

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

반응 조건

온도
92.5 °C

실험 절차

N-methyl mandelic amide 100 g, synthesized as above is dissolved in acetic anhydride 200 ml at 60 degrees C. and concentrated sulfuric acid 0.5 ml is added. The mixture is heated at 90-95 degrees C. for 5 hours to complete the acetylation. The reaction mixture is then evaporated at 70 degrees C. in vacuum and the syrupy residue thus obtained is mixed with 1 liter of ice water. Chloroform 200 ml is added to extract the oily product and the chloroform layer is washed with 5% aqueous sodium bicarbonate, 200 ml and 0.2N HCL 200 ml, and dried with anhydrous sodium sulfate. On evaporation of the chloroform solution at 40 degrees C. in vacuum white crystalline product is formed from the syrupy residue. The crystals are washed with n-hexane. N-methyl phenyl alpha-acetoxyacetamide 66 g thus synthesized is identified by infrared spectroscopy, high performance liquid chromatography and thin-layer chromatography with a mobility of 0.65 on a solvent system of benzene:methanol 1:1.

후처리

  1. customThe reaction mixture is then evaporated at 70 degrees C
  2. customin vacuum and the syrupy residue thus obtained
  3. extractionto extract the oily product
  4. washthe chloroform layer is washed with 5% aqueous sodium bicarbonate, 200 ml and 0.2N HCL 200 ml
  5. dry with materialdried with anhydrous sodium sulfate
  6. customOn evaporation of the chloroform solution at 40 degrees C
  7. customin vacuum white crystalline product is formed from the syrupy residue
  8. washThe crystals are washed with n-hexane
  9. customN-methyl phenyl alpha-acetoxyacetamide 66 g thus synthesized

출처 및 근거

ORD 기록
ord-925aaf3c2dab43bab066daab11daf5b4
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04518789

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