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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 3089143, 화합물

HRID 1599013
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인쇄 미리보기

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HRID 1599013 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].[N+:12]([C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=O)=[CH:17][CH:16]=1)([O-:14])=[O:13].O>COCCOCCOC>[N+:12]([C:15]1[CH:23]=[CH:22][C:18]([C:19]2[O:11][C:3]3[CH:4]=[CH:5][C:6]([N+:8]([O-:10])=[O:9])=[CH:7][C:2]=3[N:1]=2)=[CH:17][CH:16]=1)([O-:14])=[O:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 85024-Nitrobenzoyl chlorideHCID 36133892-Amino-4-Nitrophenol

생성물 1

HCID 3089143HCID 3089143, 화합물수율 95%

시약·촉매·용매 1

HCID 8150Diglyme용매2회

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온도
100 °C

실험 절차

2-Amino-4-nitrophenol (46.2 g, 0.3 mol) was dissolved in diglyme (1250 mL) and added to a 3-necked, 3-liter flask equipped with a condenser, a mechanical stirrer, and a hearer. 4-Nitrobenzoyl chloride (57 g, 0.3 mol) was dissolved in diglyme (250 mL) and added to the flask. The mixture was heated, with stirring, to 120° C. for 1 hour, whereupon polyphosphoric acid (90 g) was added. Heating was continued at 150° C. to 160° C. for an additional 1 hour. The reaction mixture was cooled to 110° C. to 120° C. and deionized water (500 mL) was added over a period of 15 to 30 minutes while the mixture was maintained at 100° C. The reaction mixture was cooled, and the precipitated product was filtered and washed with methanol (300 mL), then dried. The melting point was found to be 253° C. to 255° C. The overall yield was 95 percent with an assay of 100 percent by liquid chromatography.

후처리

  1. additionadded to a 3-necked, 3-liter flask
  2. customequipped with a condenser, a mechanical stirrer
  3. additionadded to the flask
  4. temperatureThe mixture was heated
  5. additionwas added
  6. temperatureHeating
  7. temperatureThe reaction mixture was cooled to 110° C. to 120° C.
  8. temperatureThe reaction mixture was cooled
  9. filtrationthe precipitated product was filtered
  10. washwashed with methanol (300 mL)
  11. customdried
  12. customto be 253° C. to 255° C

출처 및 근거

ORD 기록
ord-23dc5eb49a064112bc4c153933e57119
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05739344

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