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

HRID 1636181ノート

反応式

HRID 1636181 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0f01e2f79bae4f63b010c44d195eb930
出典データセット
uspto-grants-2003_01
特許番号
US06511993B1

反応ノート

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