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

HRID 1970707노트

반응식

HRID 1970707 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-229a898a69d64f67b84469b2eb5055a3
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08431045B2

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