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Nitrogen → 2-(2-Chloro-5-isopropenyl-pyridin-4-ylamino)-N-methyl-benzamide

HRID 62516
ノート
印刷プレビュー

反応式

HRID 62516 の反応式
N#N.Br[C:4]1[C:5]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([NH:16][CH3:17])=[O:15])=[CH:6][C:7]([Cl:10])=[N:8][CH:9]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].[C:30]1(C)[CH:35]=CC=C[CH:31]=1>O.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>[Cl:10][C:7]1[CH:6]=[C:5]([NH:11][C:12]2[CH:21]=[CH:20][CH:19]=[CH:18][C:13]=2[C:14]([NH:16][CH3:17])=[O:15])[C:4]([C:30]([CH3:35])=[CH2:31])=[CH:9][N:8]=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 4

HCID 947NitrogenHCID 1140TolueneHCID 62657Potassium Phosphate, TribasicHCID 575169042-[(5-Bromo-2-chloro-4-pyridinyl)amino]-N-methylbenzamide

生成物 1

HCID 575169072-(2-Chloro-5-isopropenyl-pyridin-4-ylamino)-N-methyl-benzamide

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

In a tube a solution of isopropenyboronic acid pinacol ester (3.31 mL, 17.6 mmole, 3 eq) in toluene (200 mL) was degassed with N2 at 50° C. for 15 min. To this was added Pd(PPh3)4 (0.68 g, 0.59 mmole, 0.1 eq) and 2-(5-bromo-2-chloro-pyridin-4-ylamino)-N-methyl-benzamide (2 g, 5.87 mmole, 1 eq). This mixture was again degassed with N2 for 30 min. A degassed solution of K3PO4 (4.98 g, 23.48 mmole, 4 eq) in H2O (8 mL) was added to the above mixture in one portion and the resulting mixture was heated at 110° C. for overnight. After completion of the reaction, it was allowed to cool to room temperature and solvent was removed under reduced pressure to yield crude product. It was purified by column chromatography over silica gel (60-120 mesh) using 0.5% MeOH-DCM as the eluant to give the title compound as an off white solid (0.8 g, 45%). 1H-NMR (400 MHz, DMSO-d6): δ 2.06 (s, 3H), 2.73-2.74 (d, 3H, J=4.52 Hz), 5.14 (s, 1H), 5.46 (s, 1H), 7.04-7.15 (m, 2H), 7.45-7.60 (m, 2H), 7.64-7.71 (m, 1H), 7.96 (s, 1H), 8.60-8.72 (brs, 1H), 9.87 (s, 1H). LC-MS [M+H]+=302.2.

後処理

  1. customThis mixture was again degassed with N2 for 30 min
  2. customAfter completion of the reaction, it
  3. temperatureto cool to room temperature
  4. customsolvent was removed under reduced pressure
  5. customto yield crude product
  6. customIt was purified by column chromatography over silica gel (60-120 mesh)

出典と根拠

ORDレコード
ord-69b4e772eb31435f9756ed06b045174c
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09446034B2

反応ノート

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