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Potassium Carbonate → 6-Chloro-5-(4-methoxyphenyl)-1H-indazole-3-carboxylic acid

HRID 338456
ノート
印刷プレビュー

反応式

HRID 338456 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][N:6]=[C:5]2[C:12]([OH:14])=[O:13].[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20](B(O)O)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CCO.C1(C)C=CC=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:11][C:10]1[CH:9]=[C:8]2[C:4]([C:5]([C:12]([OH:14])=[O:13])=[N:6][NH:7]2)=[CH:3][C:2]=1[C:20]1[CH:21]=[CH:22][C:17]([O:16][CH3:15])=[CH:18][CH:19]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 201262(4-Methoxyphenyl)boronic acidHCID 866987915-bromo-6-chloro-1H-indazole-3-carboxylic acid

生成物 1

HCID 866987906-Chloro-5-(4-methoxyphenyl)-1H-indazole-3-carboxylic acid収率 13%

試薬・触媒・溶媒 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 702Ethanol溶媒
HCID 1140Toluene溶媒

反応条件

温度
130 °C

実験手順

To a solution of 5-bromo-6-chloro-1H-indazole-3-carboxylic acid (2.0 g, 7.3 mmol), 4-methoxyphenyl boronic acid (1.13 g, 7.40 mmol) in EtOH (50 mL) and toluene (50 mL) was added 2N aqueous potassium carbonate solution (21.8 mL, 43.6 mmol). The reaction mixture was degassed with N2 for 5 minutes, treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (296 mg, 0.36 mmol) and degassed with N2 for an additional 5 minutes. The reaction mixture was sealed in a pressure tube and heated to 130° C. for 3 hours. As the reaction progressed, the suspension became clear and turned to orange then dark brown. The reaction mixture was cooled to room temperature, and filtered through Celite®. The filtrate was concentrated in vacuo and the residue was partitioned between EtOAc (150 mL) and water (150 mL). The aqueous layer was acidified to pH 2, and extracted with EtOAc. Silicycle-thiol resin was added to the organic layer and the suspension was stirred for 10 minutes. The suspension was filtered and activated charcoal was added to the filtrate. The suspension was stirred at room temperature for another 20 minutes and filtered. The resulting light yellow solution was concentrated in vacuo and the residue was triturated with CH2Cl2 and MeCN. The solid was filtered to provide the title compound (280 mg, 13% yield) as a light yellow solid. The filtrate was concentrated, diluted with EtOAc (20 mL) and filtered to give another batch of desired product (80 mg). MS (ES+) 303.2 (M+H)+. 1H NMR (500 MHz, DMSO-d6) δ 7.98 (s, 1H), 7.86 (s, 1H), 7.38 (d, J=8.29 Hz, 2H), 7.03 (d, J=8.78 Hz, 2H), 3.82 (s, 3H).

後処理

  1. customThe reaction mixture was degassed with N2 for 5 minutes
  2. customdegassed with N2 for an additional 5 minutes
  3. customThe reaction mixture was sealed in a pressure tube
  4. temperatureThe reaction mixture was cooled to room temperature
  5. filtrationfiltered through Celite®
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue was partitioned between EtOAc (150 mL) and water (150 mL)
  8. extractionextracted with EtOAc
  9. additionSilicycle-thiol resin was added to the organic layer
  10. filtrationThe suspension was filtered
  11. additionwas added to the filtrate
  12. stirringThe suspension was stirred at room temperature for another 20 minutes
  13. filtrationfiltered
  14. concentrationThe resulting light yellow solution was concentrated in vacuo
  15. customthe residue was triturated with CH2Cl2 and MeCN
  16. filtrationThe solid was filtered

出典と根拠

ORDレコード
ord-b453b35330ac4d6aaa73532c8f7c9409
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889730B2

反応ノート

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