m-Chloroperbenzoic acid → HCID 57597041, 화합물

HRID 1786155노트

반응식

HRID 1786155 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[N:18]=[C:17]2[CH2:19][CH2:20][CH2:21][C:16]2=[CH:15][CH:14]=1>C(Cl)Cl>[Cl:12][C:13]1[N+:18]([O-:9])=[C:17]2[CH2:19][CH2:20][CH2:21][C:16]2=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 150129062-Chloro-6,7-dihydro-5H-cyclopenta[b]pyridine

생성물 1

HCID 57597041HCID 57597041, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of m-chloroperbenzoic acid 70% (520.9 mg, 2.113 mmol) in 5 mL of CH2Cl2 was added drop wise to a stirring solution of 2-chloro-6,7-dihydro-5H-cyclopenta[b]pyridine (295 mg, 1.921 mmol) in 3 mL of CH2Cl2 and the resulting solution was allowed to stir at room temperature overnight. The reaction mixture was quenched with a saturated aqueous solution of NaHCO3 and the CH2Cl2 layer was separated. The aqueous phase was then extracted with CH2Cl2 (3×), and the combined organic extracts were washed with brine and then dried over anhydrous Na2SO4. After removing solvent at reduced pressure, the residue was purified by preparative TLC (eluting with 70% EtOAc/Hexane) to afford the title compound (I-1a).

후처리

  1. customThe reaction mixture was quenched with a saturated aqueous solution of NaHCO3
  2. customthe CH2Cl2 layer was separated
  3. extractionThe aqueous phase was then extracted with CH2Cl2 (3×)
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. customAfter removing solvent at reduced pressure
  7. customthe residue was purified by preparative TLC (eluting with 70% EtOAc/Hexane)

출처 및 근거

ORD 기록
ord-c65d9bf616fe48dc8db25c65061ec97e
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07507732B2

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