Aluminum(III) Chloride → Benzoic acid, 3-[(3-hydroxy-4-methoxyphenyl)(3-pyridinylmethyl)amino]-

HRID 750991ノート

反応式

HRID 750991 の反応式
C1([O:6][C:7]2[CH:8]=[C:9]([N:15]([CH2:25][C:26]3[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=3)[C:16]3[CH:17]=[C:18]([CH:22]=[CH:23][CH:24]=3)[C:19]([OH:21])=[O:20])[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])CCCC1.[Al+3].[Cl-].[Cl-].[Cl-]>C(Cl)Cl.O>[OH:6][C:7]1[CH:8]=[C:9]([N:15]([CH2:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)[C:16]2[CH:17]=[C:18]([CH:22]=[CH:23][CH:24]=2)[C:19]([OH:21])=[O:20])[CH:10]=[CH:11][C:12]=1[O:13][CH3:14]

参加物

5

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 9931830HCID 9931830、化合物

生成物 1

HCID 10360501Benzoic acid, 3-[(3-hydroxy-4-methoxyphenyl)(3-pyridinylmethyl)amino]-

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

N-(3-Cyclopentyloxy-4-methoxyphenyl)-N-(3-pyridylmethyl)-3-aminobenzoic acid (10.0 g, 23.9 mmol) was dissolved in DCM and 22.3 g (167 mmol) of AlCl3 was added. The dark brown solution stirred at room temperature overnight under N2. The reaction mixture was diluted with 100 mL of DCM and 100 mL of H2O and the pH of the aqueous phase adjusted to 5.5. The aqueous phase was extracted with 500 mL of EtOAc and the combined organic fractions were concentrated to dryness giving the desired compound.

後処理

  1. extractionThe aqueous phase was extracted with 500 mL of EtOAc
  2. concentrationthe combined organic fractions were concentrated to dryness

出典と根拠

ORDレコード
ord-067bb7e58c264b518cb45da819251713
出典データセット
uspto-grants-2008_07
特許番号
US07405230B2

反応ノート

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