Sodium Bicarbonate → HCID 67496677、化合物

HRID 1628317ノート

反応式

HRID 1628317 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:9]=[C:10](N)[CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=2)[CH:5]=[CH:4][N:3]=1.B(Br)(Br)Br.C(Cl)Cl.C([O-])(O)=[O:26].[Na+]>CO>[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:9]=[C:10]([OH:26])[CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=2)[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 22277759Boron tribromide dichloromethaneHCID 67497043HCID 67497043、化合物

生成物 1

HCID 67496677HCID 67496677、化合物収率 68%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 0° C. flask charged with 65.B (2.85 g, 11.7 mmol) was added a solution of BBr3/CH2Cl2 (1.0 M, 25 mL). The solution was allowed to warm to rt and stirred for 45 mins. The resulting mixture was treated with MeOH (7 mL), neutralized with solid NaHCO3 to PH=7 and concentrated under reduced pressure. Purification of the residue by flash chromatography on silica gel using 0-10% of MeOH/CH2Cl2 for elution gave the title product 65.C as solid (1.83 g, 68%).

後処理

  1. concentrationconcentrated under reduced pressure
  2. customPurification of the residue by flash chromatography on silica gel using 0-10% of MeOH/CH2Cl2
  3. washfor elution

出典と根拠

ORDレコード
ord-02bbece000814576a64bc6d72757e3b5
出典データセット
uspto-grants-2014_07
特許番号
US08785468B2

反応ノート

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