Sodium dichromate dihydrate → 8-Methylphenanthrene-1,10-dicarboxylic Anhydride

HRID 36632

反応式

HRID 36632 の反応式
[CH3:1][C:2]1[CH:16]=[CH:15][CH:14]=[C:13]2[C:3]=1[CH:4]=[C:5]1[C:17]3[C:8](=[CH:9][CH:10]=[CH:11][C:12]2=3)[CH:7]=[CH:6]1.[OH2:18].[OH2:19].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:21].[Na+].[Na+]>C(O)(=O)C>[CH3:1][C:2]1[CH:16]=[CH:15][CH:14]=[C:13]2[C:3]=1[CH:4]=[C:5]1[C:6]([O:19][C:7](=[O:21])[C:8]3[C:17]1=[C:12]2[CH:11]=[CH:10][CH:9]=3)=[O:18]

参加物

4

反応物 2

HCID 108005Sodium dichromate dihydrateHCID 149320397-Methylacephenanthrylene

生成物 1

HCID 537910068-Methylphenanthrene-1,10-dicarboxylic Anhydride収率 82.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A suspension of 7-methylacephenanthrylene (0.56 g, 2.59 mmol) and sodium dichromate dihydrate (2.70 g, 9.07 mmol) in glacial acetic acid (10 mL) was heated at reflux for 4 h. The reaction mixture was allowed to cool and the resulting solid was collected by suction filtration. The solid was dried to give 0.56 g (80%) of the anhydride: MS (CI) m/e (%) 263 (M+H+, 100); 1H NMR (DMSO-d6, 300 MHz) δ 9.55 (d, 1H, J=8.8 Hz), 9.04 (s, 1H), 8.89 (d, 1H, J=8.5 Hz), 8.55 (d, 1H, J=7.4 Hz), 7.75 (d, 1H, J=7.3 Hz), 2.87 (s, 3H).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 4 h
  3. temperatureto cool
  4. filtrationthe resulting solid was collected by suction filtration
  5. customThe solid was dried

出典と根拠

ORDレコード
ord-9d9be11513e849ea88d6217bb19e8c22
出典データセット
uspto-grants-1995_05
特許番号
US05416089

関連ノート

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