Triethylamine → 8-(Methanesulfonyl)-1,4-dioxa-8-azaspiro[4.5]decane

HRID 1636181노트

반응식

HRID 1636181 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]1[O:15][C:9]2([CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[O:8][CH2:7]1.C(N(CC)CC)C>CCOCC>[CH2:6]1[O:15][C:9]2([CH2:14][CH2:13][N:12]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:11][CH2:10]2)[O:8][CH2:7]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 674351,4-Dioxa-8-azaspiro(4.5)decane

생성물 1

HCID 173779138-(Methanesulfonyl)-1,4-dioxa-8-azaspiro[4.5]decane수율 95.4%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Methanesulphonyl chloride (24.8 g, 0.217mol) was added dropwise to a solution of 4-piperidone ethylene ketal (28.2 g, 0.197 mol) and triethylamine (30.2 ml, 0.217 mol) in ether (280 ml), and the reaction stirred at room temperature for 3 hours. The mixture was washed consecutively with water (2×), hydrochloric acid (1N), and saturated sodium bicarbonate solution, dried (MgSO4), filtered and evaporated in vacuo. The residue was triturated with hexane, filtered and dried to give the desired product as an off-white solid (41.6 g, 95%).

후처리

  1. washThe mixture was washed consecutively with water (2×), hydrochloric acid (1N), and saturated sodium bicarbonate solution
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was triturated with hexane
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-0f01e2f79bae4f63b010c44d195eb930
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06511993B1

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