Methyl iodide → HCID 86605588、化合物

HRID 2245335ノート

反応式

HRID 2245335 の反応式
[CH2:1]([CH:5]1[C:10](=[O:11])[CH2:9][CH2:8][N:7]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:6]1)[CH2:2][CH2:3][CH3:4].[CH3:19][I:20]>CC(C)=O>[I-:20].[CH2:12]([N+:7]1([CH3:19])[CH2:8][CH2:9][C:10](=[O:11])[CH:5]([CH2:1][CH2:2][CH2:3][CH3:4])[CH2:6]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 68684462HCID 68684462、化合物

生成物 1

HCID 86605588HCID 86605588、化合物収率 78.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 3-butyl-1-benzyl-piperidine-4-one (9080 mg) in acetone (40 ml) was slowly added methyl iodide (6303 mg) at room temperature. The solution was stirred at room temperature for three hours. A white solid precipitated and was filtered off. The solid was washed four times with 50 ml of acetone and dried under reduced pressure. The filtrate was evaporated and the residue was stirred with ethyl acetate. The white solid was filtered, washed with ethyl acetate and dried under vacuum. The two solids were combined to yield 1-benzyl-3-butyl-1-methyl-4-oxo-piperidinium iodide as a white powder (11200 mg). MS (ESI): 204.2 (M−1−).

後処理

  1. customat room temperature
  2. customA white solid precipitated
  3. filtrationwas filtered off
  4. washThe solid was washed four times with 50 ml of acetone
  5. customdried under reduced pressure
  6. customThe filtrate was evaporated
  7. stirringthe residue was stirred with ethyl acetate
  8. filtrationThe white solid was filtered
  9. washwashed with ethyl acetate
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-9ecdefaca7004e2581c65c3c8f3f0cb6
出典データセット
uspto-grants-2010_03
特許番号
US07683079B2

反応ノート

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