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1-(2-Pyrimidinyl)piperazine → HCID 17755564, 화합물

HRID 1425726
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HRID 1425726 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:14])=[CH:6][C:7]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[N:15]1[CH:20]=[CH:19][CH:18]=[N:17][C:16]=1[N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>>[CH3:14][C:5]1[N:4]=[N:3][C:2]([N:24]2[CH2:25][CH2:26][N:21]([C:16]3[N:15]=[CH:20][CH:19]=[CH:18][N:17]=3)[CH2:22][CH2:23]2)=[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 887471-(2-Pyrimidinyl)piperazineHCID 64152403-Chloro-6-methyl-4-phenylpyridazine

생성물 1

HCID 17755564HCID 17755564, 화합물수율 41.7%

실험 절차

A synthetic reaction scheme for the preparation of6-methyl-4-phenyl-3-(4-pyrimidin-2-ylpiperazin-1-yl)pyridazine (MW01-7-057) is depicted in FIG. 26, and synthesis was carried out as described herein. A mixture of 3-chloro-6-methyl-4-phenylpyridazine (100 mg, 0.5 mmol), 1-(2-pyrimidyl)piperazine (400 mg, 2.0 mmol) in 3 ml of 1-BuOH was heated with stirring at 130 C for 7 days. The solvent was removed by evaporation in vacuo, the residue was treated with water to give a suspension. The solid was then filtered off, washed with water, then 1:3, Ethyl Acetate: Petroleum ether, dried over filter funnel in vacuo to give, light yellow solid (68 mg, 0.20 mmol, yield 41.7%). Purity>95%; ESI-MS: m/z 333.1 (M+H+). 1H NMR (CDCl3): d 8.310 (d, J=5.0, 2H), 7.678 (d, J=7.5, 2H), 7.476 (m, 3H), 7.119 (s, H), 6.509 (t, J=4.5, 1H), 3.785 (t, J=4.5, J=5.0, 4H), 3.277 J=4.5, J=5.0, 4H), 2.669 (s, 3H).

후처리

  1. customA synthetic reaction scheme
  2. customis depicted in FIG. 26, and synthesis
  3. temperaturewas heated
  4. customThe solvent was removed by evaporation in vacuo
  5. additionthe residue was treated with water
  6. customto give a suspension
  7. filtrationThe solid was then filtered off
  8. washwashed with water
  9. dry with material1:3, Ethyl Acetate: Petroleum ether, dried
  10. filtrationover filter funnel in vacuo
  11. customto give

출처 및 근거

ORD 기록
ord-518a5fe586e04fdd8d81086627e8f87a
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933076B2

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