Potassium Hydroxide → N,N-Bis(pyridin-2-ylmethyl)propan-1-amine

HRID 495252

反応式

HRID 495252 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1.[OH-].[K+].I[CH2:19][CH2:20][CH3:21]>CN(C)C=O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][N:8]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)[CH2:19][CH2:20][CH3:21]

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 336431-IodopropaneHCID 73759Bis(2-pyridylmethyl)amine

生成物 1

HCID 59816448N,N-Bis(pyridin-2-ylmethyl)propan-1-amine収率 53.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a flask were added 1.0 g di-(2-picolyl)amine, 0.85 g of pulverized potassium hydroxide and 15 ml of N,N-dimethylformamide. After stirring for 1 hour under nitrogen, the mixture was cooled to 5 C and 1.7 g of 1-iodopropane were added. The mixture was heated to 35 C and stirred for 16 hours. After quenching with 30 ml water, the product was extracted with ethyl acetate and washed twice with water. Following removal of solvent, the product was purified by silica gel chromatography using ethyl acetate to give 0.65 g of a yellow oil.

後処理

  1. additionwere added
  2. temperatureThe mixture was heated to 35 C
  3. stirringstirred for 16 hours
  4. customAfter quenching with 30 ml water
  5. extractionthe product was extracted with ethyl acetate
  6. washwashed twice with water
  7. customremoval of solvent
  8. customthe product was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-8dff10f15cfe4ff69c9854119eb0a28e
出典データセット
uspto-grants-2009_05
特許番号
US07538931B2

関連ノート

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