Sodium Carbonate → 4-bromo-1-cyclopentyl-1H-pyrazole

HRID 1930390노트

반응식

HRID 1930390 반응식
C([O-])([O-])=O.[Na+].[Na+].[CH:7]1([N:12]2[CH:16]=[CH:15][CH:14]=[N:13]2)[CH2:11][CH2:10][CH2:9][CH2:8]1.[Br:17]Br>>[Br:17][C:15]1[CH:14]=[N:13][N:12]([CH:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)[CH:16]=1

참가 물질

4

반응물 3

HCID 10340Sodium CarbonateHCID 24408BromineHCID 108444351-cyclopentyl-1H-pyrazole

생성물 1

HCID 518921224-bromo-1-cyclopentyl-1H-pyrazole수율 93%

실험 절차

To a suspension of Na2CO3 (13 g, 124 mmol) in CH2OH2 (100 mL) was added 1-cyclopentyl-1 H-pyrazole (8.35 g, 62 mmol) and Br2 (3.2 mL). The resulting mixture was stirred at RT overnight. The solid was removed by filtration and the filter cake was washed with DCM. The combined filtrates were washed with water, brine and dried over anhydrous MgSO4. The solvent was concentrated to dryness to give 4-bromo-1-cyclopentyl-1 H-pyrazole (14 g, 93%). 1H NMR (300 MHz, CDCl3): δ7.46 (s, 1 H), 7.44 (s, 1 H), 4.64 (m, 1 H), 2.18-1.67(m, 8 H); MS (ESI) m/z: 215.0 [M+H]+.

후처리

  1. customThe solid was removed by filtration
  2. washthe filter cake was washed with DCM
  3. washThe combined filtrates were washed with water, brine
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationThe solvent was concentrated to dryness

출처 및 근거

ORD 기록
ord-7b1c5c2509e24f45b6a7a68fa771ec5e
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188113B2

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