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Methanol → 4-(2,4-Dichloroanilino)-7,8-dimethoxybenzo[g]quinoline-3-carbonitrile

HRID 2213723
ノート
印刷プレビュー

反応式

HRID 2213723 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[H-].[Na+].Cl[C:13]1[C:22]2[C:17](=[CH:18][C:19]3[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[CH:23][C:20]=3[CH:21]=2)[N:16]=[CH:15][C:14]=1[C:31]#[N:32].CO>CN(C=O)C.O.C(OCC)C>[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[CH:5][C:3]=1[NH:4][C:13]1[C:22]2[C:17](=[CH:18][C:19]3[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[CH:23][C:20]=3[CH:21]=2)[N:16]=[CH:15][C:14]=1[C:31]#[N:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 887MethanolHCID 111232,4-DichloroanilineHCID 24758Sodium hydrideHCID 99441164-Chloro-7,8-dimethoxybenzo[g]quinoline-3-carbonitrile

生成物 1

HCID 102959004-(2,4-Dichloroanilino)-7,8-dimethoxybenzo[g]quinoline-3-carbonitrile収率 59.5%

試薬・触媒・溶媒 3

HCID 3283
Diethyl Ether
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 178.2 mg (1.1 mmol) of 2,4-dichloroaniline and 44.0 mg (1.1 mmol) of sodium hydride in anhydrous DMF is stirred at room temperature for 0.5 hours. To the mixture is added 149.4 mg (0.5 mmol) of 4-chloro-7,8-dimethoxybenzo[g]quinoline-3-carbonitrile. The resulting mixture is heated at 50–60° C. for 1 hour. After cooling, the mixture is diluted with water and extracted with ethyl acetate. The organic phase is washed with brine and dried over sodium sulfate. Removal of the solvent yields a dark residue which is purified on preparative TLC (developing solvent: 97:3 methylene chloride/methanol), giving a yellow foam. Trituration of the foam with diethyl ether containing several drops of methanol yields 126.1 mg (59.5%) of the product as a yellow solid, mp 271–273° C.

後処理

  1. temperatureThe resulting mixture is heated at 50–60° C. for 1 hour
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe organic phase is washed with brine
  5. dry with materialdried over sodium sulfate
  6. customRemoval of the solvent
  7. customyields a dark residue which
  8. customis purified on preparative TLC (developing solvent: 97:3 methylene chloride/methanol)
  9. customgiving a yellow foam

出典と根拠

ORDレコード
ord-985c6933486047f2b25b1ae25e6a339d
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105531B2

反応ノート

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