3-Bromopentane → HCID 117988358, 화합물

HRID 2205977노트

반응식

HRID 2205977 반응식
[Br:1][C:2]1[C:6]2[C:7](=[O:11])[NH:8][CH:9]=[CH:10][C:5]=2[NH:4][CH:3]=1.[H-].[Na+].Br[CH:15]([CH2:18][CH3:19])[CH2:16][CH3:17]>CN(C=O)C>[Br:1][C:2]1[C:6]2[C:7](=[O:11])[NH:8][CH:9]=[CH:10][C:5]=2[N:4]([CH:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH:3]=1

참가 물질

5

반응물 3

HCID 157383-BromopentaneHCID 24758Sodium hydrideHCID 534125573-Bromo-1H-pyrrolo[3,2-c]pyridin-4-ol

생성물 1

HCID 117988358HCID 117988358, 화합물수율 6.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 3-bromo-1,5-dihydro-4H-pyrrolo[3,2-c]pyridin-4-one (1.00 g) in DMF (30 mL) was added sodium hydride (60% dispersion in mineral oil, 0.207 g), and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added 3-bromopentane (0.851 g), and the mixture was stirred overnight at room temperature. The reaction mixture was extracted with water and ethyl acetate, and the organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate to ethyl acetate) to give the title compound (90.5 mg).

후처리

  1. stirringthe mixture was stirred overnight at room temperature
  2. extractionThe reaction mixture was extracted with water and ethyl acetate
  3. washthe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate to ethyl acetate)

출처 및 근거

ORD 기록
ord-27c98267deb94207b4f73622c2797453
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09371320B2

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