Potassium Hydroxide → HCID 22278853、化合物

HRID 1865258ノート

反応式

HRID 1865258 の反応式
[OH-].[K+].Cl.CN.[CH2:6]([N:13]1[CH2:18][CH2:17][C:16](=O)[C:15]([CH2:21][CH3:22])([CH3:20])[CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[C:23]([BH3-])#[N:24].[Na+]>CO>[CH2:6]([N:13]1[CH2:18][CH2:17][CH:16]([NH:24][CH3:23])[C:15]([CH2:21][CH3:22])([CH3:20])[CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

6

反応物 4

HCID 14797Potassium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 6364545Methylamine hydrochlorideHCID 22278904HCID 22278904、化合物

生成物 1

HCID 22278853HCID 22278853、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium hydroxide (15.45 g, 276 mmol) was added to the stirred solution of methylamine hydrochloride (18.54 g, 276 mmol) in methanol (100 ml) and stirring was continued for 30 min at 30° C. 1-benzyl-3-ethyl-3-methyl-4-piperidinone (8 g, 34.6 mmol) was added to the resulting mixture and stirred for 6 hr. Sodium cyanoborohydride (2.18 g, 34.6 mmol) was added to it and reaction mixture was stirred for 15 hr. The reaction mixture was concentrated to dryness, triturated with water, extracted with chloroform, dried (Na2SO4) and concentrated to give 1-benzyl-4-methylamino-3-ethyl-3-methylpiperidine. Yield 6 g (67%), C16H26N2, m/z 247 (M+1).

後処理

  1. stirringstirred for 6 hr
  2. stirringwas stirred for 15 hr
  3. concentrationThe reaction mixture was concentrated to dryness
  4. customtriturated with water
  5. extractionextracted with chloroform
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-7acc88be81984d398dc8ecc04b77411d
出典データセット
uspto-grants-2009_12
特許番号
US07626032B2

反応ノート

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