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Sodium Carbonate → HCID 57537513、化合物

HRID 1693722
ノート
印刷プレビュー

反応式

HRID 1693722 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:8]([OH:14])[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])[CH:5]=[N:6][CH:7]=1.C([O-])(=O)C.[K+].Br[C:21]1[C:22]([Cl:46])=[C:23]2[C:29]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[O:36][CH3:37])=[CH:28][N:27]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:45])([CH3:44])[CH3:43])[C:24]2=[N:25][CH:26]=1.C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>CC(N(C)C)=O>[Cl:46][C:22]1[C:21]([C:2]2[CH:3]=[C:4]([CH:8]([OH:14])[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])[CH:5]=[N:6][CH:7]=2)=[CH:26][N:25]=[C:24]2[N:27]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:43])([CH3:45])[CH3:44])[CH:28]=[C:29]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[O:36][CH3:37])[C:23]=12
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 5

HCID 10340Sodium CarbonateHCID 24436Sodium SulfateHCID 517044Potassium AcetateHCID 57537472HCID 57537472、化合物HCID 57537619HCID 57537619、化合物

生成物 1

HCID 57537513HCID 57537513、化合物収率 34%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒2 回

反応条件

温度
120 °C

実験手順

A mixture of 2-(5-Bromo-pyridin-3-yl)-2-hydroxy-N,N-dimethyl-acetamide (400 mg, 1.54 mmol), bis(pinacol)diborane (431 mg, 1.7 mmol), potassium acetate (454 mg, 4.6 mmol), and 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (25 mg, 0.03 mmol) in dimethylacetamide (2 mL) was stirred under nitrogen at 120° C. for 12 h. 5-Bromo-3-(2-methoxy-phenyl)-4-chloro-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridine (491 mg, 1.05 mmol), sodium carbonate solution (2M in water, 2.3 mL, 4.6 mmol), dimethylacetamide (2 mL) and additional 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (30 mg, 0.035 mmol) was added and the mixture was stirred for an additional 2 h at 120° C. Sodium sulfate was added to the crude reaction mixture and the solids were filtered over Celite. The solids were rinsed with ethyl acetate and acetonitrile and the combined filtrate was concentrated. The resulting oil was purified by flash silica gel chromatography using a gradient of ethyl acetate in hexanes to afford 2-{5-[4-Chloro-3-(2-methoxy-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyridin-3-yl}-2-hydroxy-N,N-dimethyl-acetamide (202 mg, 0.35 mmol, 34% yield; and 2-{5-[4-Chloro-3-(2-methoxy-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyridin-3-yl}-N,N-dimethyl-acetamide.

後処理

  1. stirringthe mixture was stirred for an additional 2 h at 120° C
  2. customreaction mixture
  3. filtrationthe solids were filtered over Celite
  4. washThe solids were rinsed with ethyl acetate and acetonitrile
  5. concentrationthe combined filtrate was concentrated
  6. customThe resulting oil was purified by flash silica gel chromatography

出典と根拠

ORDレコード
ord-a06d0c937721464787117acfaa02b2dd
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158647B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート