Dimethylamine, hydrochloride → HCID 22278842、化合物

HRID 746862ノート

反応式

HRID 746862 の反応式
C([BH3-])#N.[Na+].C(OC([N:12]1[CH2:17][CH2:16][C:15](=O)[CH:14]([CH2:19][CH3:20])[CH2:13]1)=O)(C)(C)C.Cl.[CH3:22][NH:23][CH3:24].[OH-].[K+]>CO>[CH3:22][N:23]([CH3:24])[CH:15]1[CH2:16][CH2:17][NH:12][CH2:13][CH:14]1[CH2:19][CH3:20]

参加物

6

反応物 4

HCID 10473Dimethylamine, hydrochlorideHCID 14797Potassium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 22278903tert-Butyl 3-ethyl-4-oxopiperidine-1-carboxylate

生成物 1

HCID 22278842HCID 22278842、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium cyanoborohydride (3.2 g, 50.8 mmol) was added to the stirred suspension of N-tert.-butoxycarbonyl-3-ethyl-4-piperidone (8 g, 35 mmol), N,N-dimethylamine hydrochloride (14 g, 172 mmol) and KOH (9.6 g, 172 mmol) in methanol (50 ml) at 0° C. The resulting mixture was stirred for 4 hr at ambient temperature. The reaction mixture was concentrated to dryness, triturated with water, acidified with conc. HCl (pH 3˜4) and extracted with ethyl acetate to remove impurities. The aqueous layer was basified with 1 M sodium hydroxide solution (pH ˜10) and extracted with ethyl acetate. Ethyl acetate extract was dried (Na2SO4) and concentrated to dryness to give 4-dimethylamino-3-ethylpiperidine. Yield 2.3 g (37%), C9H20N2, m/z 157 (M+1).

後処理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customtriturated with water
  3. extractionextracted with ethyl acetate
  4. customto remove impurities
  5. extractionextracted with ethyl acetate
  6. extractionEthyl acetate extract
  7. dry with materialwas dried (Na2SO4)
  8. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-0f683f81cf70488087a8661dc530b58b
出典データセット
uspto-grants-2008_07
特許番号
US07393957B2

反応ノート

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