Bromide ion → 1-Boc-4-Methylenepiperidine

HRID 47338

반응식

HRID 47338 반응식
[Br-].O=[C:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1.[C:16](O[K])(C)(C)C>O1CCCC1>[CH2:16]=[C:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 259Bromide ionHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 178418922HCID 178418922, 화합물

생성물 1

HCID 27568081-Boc-4-Methylenepiperidine수율 95.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

47.2 g of methyltoluphenylphosphonium bromide and 21.9 g of tert-butyl 4-oxo-1-piperidinecarboxylate were added to a mixture of 14.8 g tert-butoxy potassium and 300 ml tetrahydrofuran, and stirred for 40 min at room temperature. The reaction solution was evaporated, diethyl ether was added thereto, and then filtered through Celite. The filtrate was washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel column chromatography to give 20.8 g of tert-butyl 4-methylene-1-piperidinecarboxylate.

후처리

  1. customThe reaction solution was evaporated
  2. additiondiethyl ether was added
  3. filtrationfiltered through Celite
  4. washThe filtrate was washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-aea03e6a9ab1404ab6329c48f4861d88
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699870B2

연결된 노트

불러오는 중…