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2,4-Dimethylaniline → HCID 12067414, 화합물

HRID 1957793
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HRID 1957793 반응식
[OH:1][C:2]1[C:11]([C:12]([OH:14])=O)=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([OH:17])=O)[CH:8]=2)[CH:3]=1.[CH3:18][C:19]1[CH:24]=[CH:23][C:22]([NH2:25])=[C:21]([CH3:26])[CH:20]=1.P(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C(C)=CC=CC=1.O>[OH:1][C:2]1[C:11]([C:12]([NH:25][C:22]2[CH:23]=[CH:24][C:19]([CH3:18])=[CH:20][C:21]=2[CH3:26])=[O:14])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([NH:25][C:22]3[CH:23]=[CH:24][C:19]([CH3:18])=[CH:20][C:21]=3[CH3:26])=[O:17])[CH:8]=2)[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 72502,4-DimethylanilineHCID 10340Sodium CarbonateHCID 24387Phosphorus trichlorideHCID 98160552-Hydroxynaphthalen-3,6-dicarboxylic acid

생성물 1

HCID 12067414HCID 12067414, 화합물수율 58.9%

시약·촉매·용매 2

HCID 962Water용매
HCID 7237O-Xylene용매

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온도
90 °C

실험 절차

2-Hydroxy-3,6-dihydroxycarbonylnaphthalene (11.6 g) and m-xylidine (13.3 g) were dispersed in xylene (232.2 g), followed by heating to 90° C. Phosphorous trichloride (6.0 g) was added dropwise at 90° to 100° C., and then the mixture was reacted at 140° C. for 3 hours. After the completion of the reaction, water (116.1 g) was added and the reaction solution was neutralized with sodium carbonate at 80° to 90° C. The solution was filtered at room temperature and washed in turn with xylene (116.1 g) and water (116.1 g). The resultant crystal was subjected to reflux washing using acetone (80 g) and then filtered. This operation was repeated three times, followed by drying to obtain 12.9 g of 2-hydroxy-3,6-bis(2,4-dimethylphenylaminocarbonyl)naphthalene as a white powdered crystal (melting point: 284.5°-286° C.).

후처리

  1. customthe mixture was reacted at 140° C. for 3 hours
  2. additionwas added
  3. filtrationThe solution was filtered at room temperature
  4. washwashed in turn with xylene (116.1 g) and water (116.1 g)
  5. temperatureto reflux
  6. washwashing
  7. filtrationfiltered
  8. customby drying

출처 및 근거

ORD 기록
ord-570a5f0061eb421b9ff5abc8b597cf1f
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05786523

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