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Dichloromethane → 3-Bromo-5-{[(2-{[3-(3-bromopropyl)phenyl]amino}-5-chloropyrimidin-4-yl)amino]methyl}phenol

HRID 1614976
ノート
印刷プレビュー

反応式

HRID 1614976 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:25]=[C:26]([O:28]C)[CH:27]=1)[CH2:5][NH:6][C:7]1[C:12]([Cl:13])=[CH:11][N:10]=[C:9]([NH:14][C:15]2[CH:16]=[C:17]([CH2:21][CH2:22][CH2:23]O)[CH:18]=[CH:19][CH:20]=2)[N:8]=1.C(Cl)Cl.B(Br)(Br)[Br:34].C([O-])(O)=O.[Na+]>C(=O)=O>[Br:1][C:2]1[CH:27]=[C:26]([OH:28])[CH:25]=[C:4]([CH2:5][NH:6][C:7]2[C:12]([Cl:13])=[CH:11][N:10]=[C:9]([NH:14][C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([CH2:21][CH2:22][CH2:23][Br:34])[CH:16]=3)[N:8]=2)[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 584678493-[3-({4-[(3-Bromo-5-methoxybenzyl)amino]-5-chloropyrimidin-2-yl}amino)phenyl]propan-1-ol

生成物 1

HCID 584679133-Bromo-5-{[(2-{[3-(3-bromopropyl)phenyl]amino}-5-chloropyrimidin-4-yl)amino]methyl}phenol収率 100%

試薬・触媒・溶媒 1

HCID 280Carbon Dioxide溶媒

実験手順

Into a reaction flask was added 3-[3-({4-[(3-bromo-5-methoxybenzyl)amino]-5-chloropyrimidin-2-yl}amino)phenyl]propan-1-ol (2.70 g, 5.65 mmol), methylene chloride (30 mL), and a solution of boron tribromide in methylene chloride (17.0 mL, 17.0 mmol, 1.0 M). The mixture was stirred at rt overnight. The resultant mixture was cooled in dry ice when NaHCO3 (saturated aqueous solution) was added. After removal of the organic solvent, the aqueous layer was extracted with methylene chloride twice. The combined organic layers were washed with water and brine successively, then dried (Na2SO4), filtered, and concentrated to give the desired product (2.97 g, 100%). LCMS for C20H19Br2ClN4O (M+H)+: m/z=526.9, 528.8.

後処理

  1. additionwas added
  2. customAfter removal of the organic solvent
  3. extractionthe aqueous layer was extracted with methylene chloride twice
  4. washThe combined organic layers were washed with water and brine successively
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-5e822ecfee594220a60729c7542c75fd
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765727B2

反応ノート

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