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4-((Morpholino)methyl)phenylboronic acid pinacol ester → 6-Bromo-3-(4-morpholin-4-ylmethylphenyl)-9H-dipyrido[2,3-b;4',3'-d]pyrrole

HRID 1506051
ノート
印刷プレビュー

反応式

HRID 1506051 の反応式
B1([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[CH:12][CH:11]=2)OC(C)(C)C(C)(C)O1.I[C:24]1[CH:37]=[N:36][C:27]2[NH:28][C:29]3[CH:34]=[N:33][C:32]([Br:35])=[CH:31][C:30]=3[C:26]=2[CH:25]=1>C(=O)([O-])[O-].[Na+].[Na+].CC1CCCO1.C(OCC)(=O)C>[Br:35][C:32]1[N:33]=[CH:34][C:29]2[NH:28][C:27]3[N:36]=[CH:37][C:24]([C:10]4[CH:11]=[CH:12][C:13]([CH2:16][N:17]5[CH2:18][CH2:19][O:20][CH2:21][CH2:22]5)=[CH:14][CH:15]=4)=[CH:25][C:26]=3[C:30]=2[CH:31]=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

6

反応物 2

HCID 27955024-((Morpholino)methyl)phenylboronic acid pinacol esterHCID 58266297HCID 58266297、化合物

生成物 1

HCID 582667156-Bromo-3-(4-morpholin-4-ylmethylphenyl)-9H-dipyrido[2,3-b;4',3'-d]pyrrole収率 30.2%

試薬・触媒・溶媒 3

HCID 73012-Methyltetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒
HCID 10340
Sodium Carbonate
溶媒

反応条件

温度
85 °C

実験手順

A degassed mixture of 4-(4-morpholinomethyl)phenylboronic acid pinacol ester (486 mg, 1.61 mmol), 3-iodo-6-bromo-9H-dipyrido[2,3-b;4′,3′-d]pyrrole (400 mg, 1.07 mmol), 1,1′-[bis(diphenylphosphino)ferrocene]dichloropalladium(II) (131 mg, 0.16 mmol) in 2N aqueous sodium carbonate solution (8 mL) and 2-methyltetrahyrdofuran (16 mL) was heated at 85° C. for 18 h. The cooled reaction mixture was diluted with ethyl acetate (100 mL) and washed with water (75 mL). The organic phase was separated, dried over sodium sulfate, filtered and evaporated in vacuo to afford a residue that was purified by flash chromatography (silica, 50 g column, Biotage, 0-15% methanol in DCM) to afford the title compound as an off-white solid (137 mg, 30%). 1H NMR (CDCl3, 300 MHz): 12.41 (s, 1H), 9.04 (d, J=2.3 Hz, 1H), 8.95 (d, J=2.3 Hz, 1H), 8.72 (d, J=1.0 Hz, 1H), 8.53 (s, 1H), 7.76 (d, J=8.0 Hz, 2H), 7.47 (d, J=8.0 Hz, 2H), 3.65-3.56 (m, 4H), 3.53 (s, 2H), 2.44-2.29 (m, 4H).

後処理

  1. customThe cooled reaction mixture
  2. washwashed with water (75 mL)
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customto afford a residue that
  8. customwas purified by flash chromatography (silica, 50 g column, Biotage, 0-15% methanol in DCM)

出典と根拠

ORDレコード
ord-76b05f6e80c7441d9f2b5d676cfcc280
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216980B2

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