m-Chloroperbenzoic acid → 5-Bromo-2-methylpyridin-1-ium-1-olate

HRID 61001

반응식

HRID 61001 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.ClC1C=CC=C(C(OO)=[O:17])C=1.C([O-])(O)=O.[Na+]>C(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N+:6]([O-:17])[CH:7]=1

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 12010205-Bromo-2-methylpyridine

생성물 1

HCID 8171645-Bromo-2-methylpyridin-1-ium-1-olate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 5-bromo-2-methylpyridine (10 g, 58.13 mmol) and meta-chloroperbenzoic acid (mCPBA, 30 g, 174.39 mmol) in CHCl3 (160 mL) was heated at 60° C. for 16 h. The mixture was cooled to rt and neutralized with satd. NaHCO3. The resulting mixture was extracted with DCM. The organic layers were combined and washed with brine and dried (MgSO4). The solvent was removed in vacuo. The crude was purified by silica gel chromatography (EtOAc/hexanes) to obtain the title compound.

후처리

  1. extractionThe resulting mixture was extracted with DCM
  2. washwashed with brine
  3. dry with materialdried (MgSO4)
  4. customThe solvent was removed in vacuo
  5. customThe crude was purified by silica gel chromatography (EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-dac80aaa1eac40c39c5b1e78352c0f96
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440982B2

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