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Aniline → HCID 10948950、化合物

HRID 1069810
ノート
印刷プレビュー

反応式

HRID 1069810 の反応式
[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.[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][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:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:14])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:17])[CH:8]=2)[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6115AnilineHCID 10340Sodium CarbonateHCID 24387Phosphorus trichlorideHCID 98160552-Hydroxynaphthalen-3,6-dicarboxylic acid

生成物 1

HCID 10948950HCID 10948950、化合物収率 45.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 7237
O-Xylene
溶媒

反応条件

温度
90 °C

実験手順

2-Hydroxy-3,6-dihydroxycarbonylnaphthalene (4.64 g) and aniline (4.10 g) were dispersed in xylene (92.8 g), followed by heating to 90° C. Phosphorous trichloride (2.4 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 (92.8 g) was added and the reaction solution was neutralized with sodium carbonate at 90° C. The solution was filtered at room temperature and washed in turn with xylene (46.4 g) and water (46.4 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 3.5 g of 2-hydroxy-3,6-diphenylaminocarbonylnaphthalene as a white powdered crystal (melting point: 314-317° C.).

後処理

  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 (46.4 g) and water (46.4 g)
  5. temperatureto reflux
  6. washwashing
  7. filtrationfiltered
  8. customby drying

出典と根拠

ORDレコード
ord-0a07a9482a8846e0a1f9cb90a2e248cb
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06252104B1

反応ノート

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