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Sodium Carbonate → 1-[3-(2-Ethoxy-3,5-diisopropyl-phenyl)-thieno[2,3-c]pyridin-5-yl]-ethanone

HRID 1394637
ノート
印刷プレビュー

反応式

HRID 1394637 の反応式
[CH2:1]([O:3][C:4]1[C:9]([CH:10]([CH3:12])[CH3:11])=[CH:8][C:7]([CH:13]([CH3:15])[CH3:14])=[CH:6][C:5]=1B(O)O)[CH3:2].Br[C:20]1[C:28]2[C:23](=[CH:24][N:25]=[C:26]([C:29](=[O:31])[CH3:30])[CH:27]=2)[S:22][CH:21]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.[Cl-].[Na+].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>[CH2:1]([O:3][C:4]1[C:9]([CH:10]([CH3:12])[CH3:11])=[CH:8][C:7]([CH:13]([CH3:15])[CH3:14])=[CH:6][C:5]=1[C:20]1[C:28]2[C:23](=[CH:24][N:25]=[C:26]([C:29](=[O:31])[CH3:30])[CH:27]=2)[S:22][CH:21]=1)[CH3:2]
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 10340Sodium CarbonateHCID 179527371-(3-Bromo-thieno[2,3-c]pyridin-5-yl)-ethanoneHCID 18504242(2-Ethoxy-3,5-diisopropylphenyl)-boronic acid

生成物 1

HCID 596820741-[3-(2-Ethoxy-3,5-diisopropyl-phenyl)-thieno[2,3-c]pyridin-5-yl]-ethanone収率 91.5%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 1140Toluene溶媒
HCID 57417360Sodium chloride; water溶媒

反応条件

温度
90 °C

実験手順

2-Ethoxy-3,5-diisopropyl-phenyl-boronic acid (586 mg, 2.34 mmol) was dissolved in toluene (10 ml). 1-(3-Bromo-thieno[2,3-c]pyridin-5-yl)-ethanone (310 mg, 1.21 mmol), and tetrakis(triphenylphosphine)palladium(0) (140 mg, 0.12 mmol) followed by 2M sodium carbonate solution (2.34 ml) was added to this solution. This mixture was then heated to 90° C. overnight, then poured into brine (20 ml) and extracted with ethyl acetate (2×20 mL). The organic layers were dried over MgSO4 and concentrated in vacuo. The residue was then purified by chromatography (chromatotron, 4μ plate, 10% ethyl acetate in hexanes) to give a 1-[3-(2-ethoxy-3,5-diisopropyl-phenyl)-thieno[2,3-c]pyridin-5-yl]-ethanone as a white solid (422.2 mg, 91%). 1H NMR (250 MHz, CDCl3): δ 9.14 (s, 1H), 8.38 (s, 1H), 7.80 (s, 1H), 7.13 (d, 1H, J=1.9), 6.98 (d, 1H, J=1.9), 3.33 (m, 1H), 3.28 (q, 2H, J=7.5), 2.87 (m, 1H), 2.74 (s, 3H), 1.25 (s, 3H), 1.23 (s, 3H), 1.22 (s, 3H), 1.20 (s, 3H), 0.85 (t, 3H, J=7.5). MS [EI+] 382 (M+H)+.

後処理

  1. additionwas added to this solution
  2. extractionextracted with ethyl acetate (2×20 mL)
  3. dry with materialThe organic layers were dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was then purified by chromatography (chromatotron, 4μ plate, 10% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-779ddee85f73464fbc788776fbee42ab
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07348359B2

反応ノート

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