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

HRID 1930390ノート

反応式

HRID 1930390 の反応式
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

参加物

4

反応物 3

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

生成物 1

HCID 518921224-bromo-1-cyclopentyl-1H-pyrazole収率 93%

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-7b1c5c2509e24f45b6a7a68fa771ec5e
出典データセット
uspto-grants-2012_05
特許番号
US08188113B2

反応ノート

読み込み中…