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Methylboronic Acid → 4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester

HRID 2411202
ノート
印刷プレビュー

反応式

HRID 2411202 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2C(Cl)=CC(Cl)=C[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1(P(C2CCCCC2)C2C=CC=C[C:30]=2[C:35]2[C:40](OC)=C[CH:38]=[CH:37][C:36]=2OC)CCCCC1.[F-].[K+].CB(O)O>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[C:37]([CH3:38])=[CH:36][C:35]([CH3:30])=[CH:40][N:15]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 139377Methylboronic AcidHCID 522689Potassium FluorideHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 67380983Tert-butyl 4-(3,5-dichloropyridin-2-yl)piperazine-1-carboxylate

生成物 1

HCID 673812824-(3,5-Dimethylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester収率 449%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 2,3,5-trichloropyridine (25 g), 1-Boc-piperazine (28.13 g) and potassium carbonate (37.86 g) were added N,N-dimethylformamide (25 mL) and toluene (50 mL), and the mixture was stirred at 100° C. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give 4-(3,5-dichloropyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (39.13 g). To a mixture of the obtained 4-(3,5-dichloropyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (6.35 g), palladium(II) acetate (0.46 g), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (1.71 g), potassium fluoride (9.56 g) and methylboronic acid (5 g) was added tetrahydrofuran (202 mL), and the mixture was stirred with heating under reflux for 8 hr under a nitrogen stream. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give 4-(3,5-dimethylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (5.45 g). The obtained 4-(3,5-dimethylpyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (5.45 g) was dissolved in chloroform (46 mL), 4N hydrogen chloride/ethyl acetate (18 ml) was added, and the mixture was stirred at room temperature. After completion of the reaction, to the reaction mixture were added water and potassium carbonate, the mixture was extracted with ethyl acetate, and the solvent was evaporated to give the title compound (3.3 g).

後処理

  1. temperaturewith heating
  2. temperatureunder reflux for 8 hr under a nitrogen stream
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. customthe solvent was evaporated
  6. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-6219351b06d447c086eb633cb681746a
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

反応ノート

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