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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Anhydride → HCID 19003304, 화합물

HRID 2255733
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HRID 2255733 반응식
[CH3:1][C:2]1([CH3:26])[CH2:7][CH:6]([N:8]2[C:12](=[O:13])[C:11]3=[CH:14][C:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:16][CH:17]=[C:10]3[C:9]2=[O:23])[CH2:5][C:4]([CH3:25])([CH3:24])[NH:3]1.[C:27](OC(=O)C)(=[O:29])[CH3:28]>CN(C)C1C=CN=CC=1>[C:27]([N:3]1[C:4]([CH3:25])([CH3:24])[CH2:5][CH:6]([N:8]2[C:12](=[O:13])[C:11]3=[CH:14][C:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:16][CH:17]=[C:10]3[C:9]2=[O:23])[CH2:7][C:2]1([CH3:1])[CH3:26])(=[O:29])[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 19003301HCID 19003301, 화합물

생성물 1

HCID 19003304HCID 19003304, 화합물

시약·촉매·용매 1

HCID 142844-(Dimethylamino)pyridine촉매

실험 절차

Into a 125 ml reaction flask equipped with a magnetic stirrer, thermometer, condenser and nitrogen atmosphere were placed the HALS of Example 4 (0.9 g, 0.0025 mol), 4-dimethylaminopyridine (0.03 g) and 25 ml of acetic anhydride. The reaction was refluxed for 2 hours, then poured into a beaker containing 200 ml ice water. A brown oil separated immediately and the mixture was stirred until the oil solidified into a tan solid. This solid was isolated by filtration and washed on the filter funnel with several portions of water. The wet solid was dissolved in 50 ml methylene chloride and dried with anhydrous magnesium sulfate. The solvent was stripped to give 0.9 g of light tan crystals melting at 119°-121° C. The infrared spectrum (in chloroform) showed a broad carbonyl absorption at 1710 cm-1 (imide and ester) and an amide carbonyl at 1615 cm-1.

후처리

  1. customInto a 125 ml reaction flask
  2. customequipped with a magnetic stirrer
  3. customthermometer, condenser and nitrogen atmosphere were placed
  4. temperatureThe reaction was refluxed for 2 hours
  5. additionpoured into a beaker
  6. customA brown oil separated immediately
  7. customThis solid was isolated by filtration
  8. washwashed on the filter funnel with several portions of water
  9. dissolutionThe wet solid was dissolved in 50 ml methylene chloride
  10. dry with materialdried with anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-5ef154e3728d4510ae309a20969737e8
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05241067

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