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Phloroglucinol → HCID 10540475, 화합물

HRID 478682
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HRID 478682 반응식
[NH2:1][C:2]1[C:3]([C:12]([OH:14])=O)=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[OH:15][C:16]1[CH:21]=[C:20](O)[CH:19]=[C:18]([OH:23])[CH:17]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)CCCCCC>[OH:15][C:16]1[C:21]2[C:12](=[O:14])[C:3]3[CH:4]=[C:5]4[CH:6]=[CH:7][CH:8]=[CH:9][C:10]4=[CH:11][C:2]=3[NH:1][C:20]=2[CH:19]=[C:18]([OH:23])[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 359PhloroglucinolHCID 6101p-Toluenesulfonic acidHCID 222443-Amino-2-naphthoic acid

생성물 1

HCID 10540475HCID 10540475, 화합물

시약·촉매·용매 1

HCID 8129Heptanol용매

실험 절차

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

후처리

  1. temperatureunder reflux
  2. concentrationthe reaction mixture is then concentrated in vacuo
  3. customThe residue is chromatographed over silica gel (eluant:cyclohexane/acetone: 90/10)
  4. customThe isolated product is crystallised from a cyclohexane/acetone mixture
  5. customto be obtained

출처 및 근거

ORD 기록
ord-e4144cce5a6d4a16b18734d3fe869d9c
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06642248B2

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