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Trifluoroacetic anhydride → 6-Methoxy-3,3-dimethyl-13-nitro-3,14-dihydro-7H-benzo[b]pyrano[3,2-h]-acridin-7-one

HRID 478690
ノート
印刷プレビュー

反応式

HRID 478690 の反応式
[CH3:1][C:2]1([CH3:31])[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][C:6]([O:29][CH3:30])=[CH:7][C:8]=2[NH:12][C:13]2[C:14]([C:26]([OH:28])=O)=[CH:15][C:16]3[C:21]([C:22]=2[N+:23]([O-:25])=[O:24])=[CH:20][CH:19]=[CH:18][CH:17]=3)[O:3]1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>ClCCl>[CH3:30][O:29][C:6]1[CH:5]=[C:4]2[O:3][C:2]([CH3:1])([CH3:31])[CH:11]=[CH:10][C:9]2=[C:8]2[C:7]=1[C:26](=[O:28])[C:14]1[CH:15]=[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:21]3=[C:22]([N+:23]([O-:25])=[O:24])[C:13]=1[NH:12]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9845Trifluoroacetic anhydrideHCID 220645353-[(2,2-Dimethyl-7-methoxy-2H-chromen-5-yl)amino]-4-nitro-2-naphthalene-carboxylic acid

生成物 1

HCID 220645196-Methoxy-3,3-dimethyl-13-nitro-3,14-dihydro-7H-benzo[b]pyrano[3,2-h]-acridin-7-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

772 mg of the compound obtained in Step 4 are dissolved in 45 ml of anhydrous dichloromethane, and 3 ml of trifluoroacetic anhydride are added. After stirring for 5 minutes at ambient temperature, the reaction mixture is evaporated. The residue is taken up in a mixture of dichloromethane and saturated NaHCO3 solution. After extraction of the aqueous phase with dichloromethane, the combined organic phases are treated in conventional manner and then distilled, allowing the expected product to be isolated.

後処理

  1. customthe reaction mixture is evaporated
  2. additionThe residue is taken up in a mixture of dichloromethane and saturated NaHCO3 solution
  3. extractionAfter extraction of the aqueous phase with dichloromethane
  4. additionthe combined organic phases are treated in conventional manner
  5. distillationdistilled
  6. customto be isolated

出典と根拠

ORDレコード
ord-3f605cc6caf441aea8ea3a873c713991
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06642248B2

反応ノート

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