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Sodium Carbonate → HCID 57537662、化合物

HRID 1693721
ノート
印刷プレビュー

反応式

HRID 1693721 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]([C:46]([F:49])([F:48])[F:47])=[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](COCC[Si](C)(C)C)[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>[OH:14][CH:8]([C:4]1[CH:5]=[N:6][CH:7]=[C:2]([C:21]2[C:22]([C:46]([F:47])([F:48])[F:49])=[C:23]3[C:29]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=4[O:36][CH3:37])=[CH:28][NH:27][C:24]3=[N:25][CH:26]=2)[CH:3]=1)[C:9]([N:11]([CH3:13])[CH3:12])=[O:10]
参加物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 57537548HCID 57537548、化合物HCID 57537619HCID 57537619、化合物

生成物 1

HCID 57537662HCID 57537662、化合物収率 7%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A mixture of 2-(5-Bromo-pyridin-3-yl)-2-hydroxy-N,N-dimethyl-acetamide (40 mg, 0.15 mmol), bis(pinacol)diborane (47 mg, 0.18 mmol), potassium acetate (45 mg, 0.46 mmol), and 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (6 mg, 0.007 mmol) in dimethylacetamide (1 mL) was irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min. 5-Bromo-3-(2-methoxy-phenyl)-4-trifluoromethyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridine (39 mg, 0.077 mmol), sodium carbonate solution (2M in water, 0.39 mL, 0.77 mmol), and additional 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (3 mg, 0.03 mmol) was added and the mixture was irradiated for an additional 30 min 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 the combined filtrate was concentrated. The solids were resuspended in ethyl acetate, filtered through a plug of silica and the eluent was concentrated. The resulting oil was dissolved in trifluoroacetic acid (2 mL) and shaken for 5 min. The solution was concentrated and the mixture was redissolved in dimethyl sulfoxide and ethylenediamine. Purification by mass triggered reverse phase HPLC afforded 2-Hydroxy-2-{5-[3-(2-methoxy-phenyl)-4-trifluoromethyl-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyridin-3-yl}-N,N-dimethyl-acetamide (2.5 mg, 0.005 mmol, 7% yield). 1H NMR (500 MHz, MeOH-d4) δ 12.55 (bs, 1H), 8.60 (s, 1H), 8.51 (s, 1H), 8.24 (s, 1H), 7.72 (s, 1H), 7.71 (m, 1H), 7.31 (m, 1H), 7.24 (dd, J=7 Hz, J2=2 Hz, 1H), 6.99 (d, J=7.5 Hz, 1H), 6.95 (td, J=7.5 Hz, J2=1 Hz, 1H), 5.8 (bs, 1H), 5.56 (s, 1H), 3.65 (s, 3H), 2.90 (m, 3H), 2.84 (s, 3H). MS: m/z 471.0 (M+H+).

後処理

  1. customwas irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min
  2. customthe mixture was irradiated for an additional 30 min at 120° C
  3. customreaction mixture
  4. filtrationthe solids were filtered over Celite
  5. washThe solids were rinsed with ethyl acetate
  6. concentrationthe combined filtrate was concentrated
  7. filtrationfiltered through a plug of silica
  8. concentrationthe eluent was concentrated
  9. dissolutionThe resulting oil was dissolved in trifluoroacetic acid (2 mL)
  10. concentrationThe solution was concentrated
  11. dissolutionthe mixture was redissolved in dimethyl sulfoxide
  12. customPurification by mass triggered reverse phase HPLC

出典と根拠

ORDレコード
ord-e887dd6a627c40ba8143286cb8aaab47
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実験手順後処理出典と根拠反応ノート