Bromine → Tert-butyl 4-(5-bromo-3-formylpyridin-2-yl)piperazine-1-carboxylate

HRID 2403611노트

반응식

HRID 2403611 반응식
[CH:1]([C:3]1[C:4]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)=[N:5][CH:6]=[CH:7][CH:8]=1)=[O:2].[Br:22]Br>C(O)(=O)C>[Br:22][C:7]1[CH:8]=[C:3]([CH:1]=[O:2])[C:4]([N:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:13][CH2:14]2)=[N:5][CH:6]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 24741846tert-Butyl 4-(3-formylpyridin-2-yl)piperazine-1-carboxylate

생성물 1

HCID 86667973Tert-butyl 4-(5-bromo-3-formylpyridin-2-yl)piperazine-1-carboxylate수율 85.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

tert-Butyl 4-(3-formylpyridin-2-yl)piperazine-1-carboxylate (1.88 g) was dissolved in acetic acid (20 ml), and bromine (1.03 g) was added dropwise thereto, followed by stirring at room temperature for 30 minutes. The solvent was evaporated under reduced pressure. The obtained residue was subjected to liquid separation by the addition of CHCl3 and a 1 M aqueous NaOH solution. The organic layer was dried over MgSO4 and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain tert-butyl 4-(5-bromo-3-formylpyridin-2-yl)piperazine-1-carboxylate (2.05 g).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customThe obtained residue was subjected to liquid separation by the addition of CHCl3
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a7c00c3c7fd14f74b1487e90acee8a11
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802679B2

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