홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

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

HRID 1526158
노트
인쇄 미리보기

반응식

HRID 1526158 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

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

생성물 1

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

시약·촉매·용매

4
HCID 74236Tetrabutylammonium Bromide촉매HCID 167845palladium(II) acetate촉매HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-20244e6486ef41158c45c3e3d958b5b1
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09085579B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트