ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

2,4-Dimethylaniline → HCID 12067414、化合物

HRID 1957793
ノート
印刷プレビュー

反応式

HRID 1957793 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.[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
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 72502,4-DimethylanilineHCID 10340Sodium CarbonateHCID 24387Phosphorus trichlorideHCID 98160552-Hydroxynaphthalen-3,6-dicarboxylic acid

生成物 1

HCID 12067414HCID 12067414、化合物収率 58.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 7237O-Xylene溶媒

反応条件

温度
90 °C

実験手順

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.).

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 (116.1 g) and water (116.1 g)
  5. temperatureto reflux
  6. washwashing
  7. filtrationfiltered
  8. customby drying

出典と根拠

ORDレコード
ord-570a5f0061eb421b9ff5abc8b597cf1f
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05786523

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート