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Sodium Carbonate → 3-(2-Aminonaphthalen-1-yl)benzoic acid

HRID 1526158
ノート
印刷プレビュー

反応式

HRID 1526158 の反応式
C(=O)([O-])[O-].[Na+].[Na+].O.O.[Na].[Na].C(N(CC(O)=O)CC(O)=O)CN(CC(O)=O)CC(O)=O.Br[C:32]1[C:41]2[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH:35]=[CH:34][C:33]=1[NH2:42].[C:43]([C:46]1[CH:47]=[C:48](B(O)O)[CH:49]=[CH:50][CH:51]=1)([OH:45])=[O:44].C(=O)([O-])[O-].[K+].[K+]>O.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(O)(=O)C>[NH2:42][C:33]1[CH:34]=[CH:35][C:36]2[C:41](=[CH:40][CH:39]=[CH:38][CH:37]=2)[C:32]=1[C:50]1[CH:51]=[C:46]([CH:47]=[CH:48][CH:49]=1)[C:43]([OH:45])=[O:44]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 27339573-Carboxyphenylboronic acidHCID 108678611-Bromonaphthalen-2-amineHCID 86660564Disodium ethylenediaminetetraacetic acid dihydrate

生成物 1

HCID 585687123-(2-Aminonaphthalen-1-yl)benzoic acid

試薬・触媒・溶媒

4
HCID 74236Tetrabutylammonium Bromide触媒HCID 167845palladium(II) acetate触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

A freshly prepared solution of 112 mg (0.5 mmol) of palladium(II) acetate, 106 mg (1 mmol) of sodium carbonate and 186 mg (0.5 mmol) of ethylenediaminetetraacetic acid disodium dihydrate in 50 ml of water is added to a vigorously stirred mixture of 22.2 g (100 mmol) of 1-bromo-2-aminonaphthalene [20191-75-7], 18.3 g (110 mmol) of 3-carboxybenzeneboronic acid [25487-66-5], 27.6 g (200 mmol) of potassium carbonate and 645 mg (2 mmol) of tetrabutylammonium bromide in 300 ml of water, and the mixture is heated under reflux for 16 h. After cooling, the pH is adjusted to 3-4 by addition of acetic acid, and the solid is filtered off with suction, washed a number of times with 5% by weight acetic acid, dried in vacuo and then subjected to azeotropic drying with toluene. Yield: 23.8 g (90 mmol), 90.4%; purity according to 1H-NMR about 98%.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 16 h
  3. temperatureAfter cooling
  4. filtrationthe solid is filtered off with suction
  5. washwashed a number of times with 5% by weight acetic acid
  6. customdried in vacuo
  7. dry with materialto azeotropic drying with toluene

出典と根拠

ORDレコード
ord-20244e6486ef41158c45c3e3d958b5b1
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09085579B2

反応ノート

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