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

HRID 1070698

反応式

HRID 1070698 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 hours. 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-c9f3ab24e3d249ab9e8e55d965ecc83a
出典データセット
uspto-grants-2005_06
特許番号
US06903117B2

関連ノート

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