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Sodium Carbonate → 4-Chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid methyl ester

HRID 448891
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HRID 448891 반응식
Br[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[CH3:10][O:11][C:12](=[O:29])[C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15](B2OC(C)(C)C(C)(C)O2)[CH:14]=1.C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:10][O:11][C:12](=[O:29])[C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([C:2]2[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=2)[CH:14]=1
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 8170902-Bromo-3,5-dichloropyridineHCID 20816364Methyl 4-chloro-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate

생성물 1

HCID 686021224-Chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid methyl ester수율 94.8%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 21863594Toluene ethanol용매

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온도
90 °C

실험 절차

A mixture of 2-bromo-3,5-dichloropyridine (2.72 g, 12 mmol), 4-chloro-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzoic acid methyl ester (1.78 g, 6 mmol)), 2N Na2CO3 (9.0 mL, 18 mmol), Pd(PPh3)4 (0.35 g, 0.3 mmol) in toluene/ethanol (30 mL/6 mL) was sealed and heated at 90° C. for 12 hrs. The mixture was concentrated and partitioned between ethyl acetate and water. The ethyl acetate layer was washed with water and brine and was dried over MgSO4. After filtration and concentration, purification by silica gel chromatography eluting with ethyl acetate/hexane (5/95) gave 4-chloro-3-(3,5-dichloro-pyridin-2-yl)-benzoic acid methyl ester (1.8 g). MS (M+H)+: 315.6, tR=8.505 min (method 2)

후처리

  1. customwas sealed
  2. concentrationThe mixture was concentrated
  3. custompartitioned between ethyl acetate and water
  4. washThe ethyl acetate layer was washed with water and brine
  5. dry with materialwas dried over MgSO4
  6. filtrationAfter filtration and concentration, purification by silica gel chromatography
  7. washeluting with ethyl acetate/hexane (5/95)

출처 및 근거

ORD 기록
ord-a71abc9bde874b62bb4422e26d57aa6b
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481738B2

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