Water → N1-(6-chloropyrimidin-4-yl)-N3,N3-dimethylpropane-1,3-diamine

HRID 58153노트

반응식

HRID 58153 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH3:18][N:19]([CH3:24])[CH2:20][CH2:21][CH2:22][NH2:23].O>CC(O)C>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH:23][CH2:22][CH2:21][CH2:20][N:19]([CH3:24])[CH3:18])[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7993N,N-Dimethyl-1,3-propanediamineHCID 709434,6-DichloropyrimidineHCID 81531Diisopropylethylamine

생성물 1

HCID 56832157N1-(6-chloropyrimidin-4-yl)-N3,N3-dimethylpropane-1,3-diamine수율 80%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a solution of 4,6-dichloro-pyrimidine (1 g, 6.7 mmol) and DIPEA (1.03 g, 8 mmol) in iPrOH (20 mL) was added N,N-dimethyl-propane-1,3-diamine (714 g, 7 mmol) at room temperature. The resulting mixture was stirred for 2 hours. Water was added and the mixture was extracted with DCM. The combined extracts were washed with brine, dried over anhydrous Na2SO4, and concentrated to give the crude product, which was purified by flash chromatography on silica to obtain the title compound (1.15 g, yield: 80%). MS (ESI): 215 [M+H]+.

후처리

  1. extractionthe mixture was extracted with DCM
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customto give the crude product, which
  6. customwas purified by flash chromatography on silica

출처 및 근거

ORD 기록
ord-3ee391e11dbd4aecab3a79922157b754
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434697B2

반응 노트

불러오는 중…