Methyl iodide → 1,2,2,6,6-Pentamethyl-4-piperidone hydroiodide

HRID 377366

反応式

HRID 377366 の反応式
O.[CH3:2][C:3]1([CH3:12])[CH2:8][C:7](=[O:9])[CH2:6][C:5]([CH3:11])([CH3:10])[NH:4]1.[CH3:13][I:14]>C(O)(C)C>[IH:14].[CH3:13][N:4]1[C:5]([CH3:11])([CH3:10])[CH2:6][C:7](=[O:9])[CH2:8][C:3]1([CH3:12])[CH3:2]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 223976024-Piperidinone, 2,2,6,6-tetramethyl-, monohydrate

生成物 1

HCID 223975731,2,2,6,6-Pentamethyl-4-piperidone hydroiodide収率 46%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A solution of 2,2,6,6-tetramethyl-4-piperidone monohydrate (40 g, 23.1 mmol) and methyl iodide (98.31 g, 69.3 mmol) in isopropyl alcohol (25 mL) was stirred at RT for 48 h. The resulting suspension was filtered, the solid residue was dried and recrystallized from MeOH. After filtration and repeated washings with MeOH the solid was dried giving pure title compound (31.6 g, 10.6 mmol, yield 46.0%) as pale brown crystals.

後処理

  1. filtrationThe resulting suspension was filtered
  2. customthe solid residue was dried
  3. customrecrystallized from MeOH
  4. filtrationAfter filtration
  5. washwashings with MeOH the solid
  6. customwas dried

出典と根拠

ORDレコード
ord-eae7e283f1c043a3a0d4c9e0ca3c482b
出典データセット
uspto-grants-2000_02
特許番号
US06025390

関連ノート

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