Triethylamine → 3-[(8-Methoxy-2,2-dimethyl-2H-chromen-5-yl)amino]-2-naphthoic acid

HRID 1827909ノート

反応式

HRID 1827909 の反応式
Br[C:2]1[C:3]([C:12]([OH:14])=[O:13])=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.CO[C:17]1[CH:28]=[C:27]([NH2:29])[C:20]2[CH:21]=[CH:22][C:23]([CH3:26])([CH3:25])[O:24][C:19]=2[CH:18]=1.[C:30]([O-])(=[O:32])C.[K+].C(N(CC)CC)C>CC(O)C.CC([O-])=O.CC([O-])=O.[Cu+2].O.ClCCl>[CH3:30][O:32][C:18]1[CH:17]=[CH:28][C:27]([NH:29][C:2]2[C:3]([C:12]([OH:14])=[O:13])=[CH:4][C:5]3[C:10]([CH:11]=2)=[CH:9][CH:8]=[CH:7][CH:6]=3)=[C:20]2[C:19]=1[O:24][C:23]([CH3:25])([CH3:26])[CH:22]=[CH:21]2

参加物

8

反応物 4

HCID 8471TriethylamineHCID 517044Potassium AcetateHCID 109981537-methoxy-2,2-dimethyl-2H-1-benzopyran-5-ylamineHCID 122263533-Bromonaphthalene-2-carboxylic acid

生成物 1

HCID 220645103-[(8-Methoxy-2,2-dimethyl-2H-chromen-5-yl)amino]-2-naphthoic acid

試薬・触媒・溶媒 3

HCID 165397Cupric acetate monohydrate触媒HCID 3776Isopropanol溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution containing 1.2 mmol of 3-bromonaphthalene-2-carboxylic acid, 1.19 mmol of 7-methoxy-2,2-dimethyl-2H-1-benzopyran-5-ylamine, 2.38 mmol of potassium acetate, 10 mg of Cu(OAc)2.H2O and 1.19 mmol of triethylamine in 17 ml of 2-propanol is refluxed for 24 hours and then concentrated under reduced pressure. The residue obtained is taken up in a 2/1 mixture of dichloromethane/1N HCl. The aqueous phase is extracted with dichloromethane and the combined organic phases are then treated in conventional manner. Chromatography of the residue over silica gel (dichloromethane) allows the expected product to be isolated.

後処理

  1. temperatureis refluxed for 24 hours
  2. concentrationconcentrated under reduced pressure
  3. customThe residue obtained
  4. extractionThe aqueous phase is extracted with dichloromethane
  5. additionthe combined organic phases are then treated in conventional manner
  6. customto be isolated

出典と根拠

ORDレコード
ord-63a5dc39d4384789b3f8d57f08f0f2df
出典データセット
uspto-grants-2006_06
特許番号
US07056929B2

反応ノート

読み込み中…