Sodium Bicarbonate → HCID 67496677, 화합물

HRID 1628317노트

반응식

HRID 1628317 반응식
[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

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 22277759Boron tribromide dichloromethaneHCID 67497043HCID 67497043, 화합물

생성물 1

HCID 67496677HCID 67496677, 화합물수율 68%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-02bbece000814576a64bc6d72757e3b5
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785468B2

반응 노트

불러오는 중…