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Phloroglucinol → HCID 10540475, 화합물

HRID 1595208
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HRID 1595208 반응식
O[C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[CH:3]=1.[NH2:10][C:11]1[C:12]([C:21](O)=[O:22])=[CH:13][C:14]2[C:19]([CH:20]=1)=[CH:18][CH:17]=[CH:16][CH:15]=2>C(O)CCCCCC.C1(C)C=CC(S(O)(=O)=O)=CC=1>[OH:8][C:6]1[C:7]2[C:21](=[O:22])[C:12]3[CH:13]=[C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:19]4=[CH:20][C:11]=3[NH:10][C:2]=2[CH:3]=[C:4]([OH:9])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 359PhloroglucinolHCID 222443-Amino-2-naphthoic acid

생성물 1

HCID 10540475HCID 10540475, 화합물수율 70.2%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 8129Heptanol용매

실험 절차

3.5 g of 1,3,5-trihydroxybenzene and 62.5 mg of para-toluenesulphonic acid are added to a solution of 5 g of 3-amino-2-naphthalenecarboxylic acid in 50 ml of heptan-1-ol. The mixture is maintained at reflux using a Dean-Stark apparatus for 48 hours, with stirring, and the reaction mixture is then concentrated in vacuo. The residue is chromatographed on silica gel (eluant: cyclohexane/acetone: 90/10). The isolated product is crystallised from a cyclohexane/acetone mixture, yielding 5.2 g of the expected product.

후처리

  1. temperatureThe mixture is maintained
  2. temperatureat reflux
  3. customfor 48 hours
  4. concentrationthe reaction mixture is then concentrated in vacuo
  5. customThe residue is chromatographed on silica gel (eluant: cyclohexane/acetone: 90/10)
  6. customThe isolated product is crystallised from a cyclohexane/acetone mixture

출처 및 근거

ORD 기록
ord-0be4b1a6d833476cbdaa5e0894292c91
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06288073B1

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