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Dimethylamine → 2-N-{4-[3-(dimethylamino)-2-hydroxypropoxy]phenyl}-4-N-phenylpyrimidine-2,4-diamine

HRID 347754
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HRID 347754 반응식
[NH:1]([C:8]1[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH:23]3[O:25][CH2:24]3)=[CH:17][CH:16]=2)[N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:26][NH:27][CH3:28]>CN(C=O)C.CCO>[CH3:26][N:27]([CH2:24][CH:23]([OH:25])[CH2:22][O:21][C:18]1[CH:17]=[CH:16][C:15]([NH:14][C:10]2[N:9]=[C:8]([NH:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH:13]=[CH:12][N:11]=2)=[CH:20][CH:19]=1)[CH3:28]
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참가 물질

5

반응물 2

HCID 674DimethylamineHCID 179811334-Anilino-2-(4-(2,3-epoxypropoxy)anilino)pyrimidine

생성물 1

HCID 65389852-N-{4-[3-(dimethylamino)-2-hydroxypropoxy]phenyl}-4-N-phenylpyrimidine-2,4-diamine수율 18%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6228Dimethylformamide용매

실험 절차

4-Anilino-2-(4-(2,3-epoxypropoxy)anilino)pyrimidine (Reference Example I-1, 0.61 g, 1.84 mmol) was dissolved in DMF (2 ml) and treated with dimethylamine (6 mmol, 3 ml of a 2M solution in EtOH). After stirring overnight at ambient temperature the reaction mixture was partitioned between EtOAc and water. The organic phase was washed with water, dried over MgSO4 and evaporated at reduced pressure. The residue was purified by chromatography (0.1%NH3 (aq), 3–10% MeOH in DCM as eluent). Upon evaporation of the fractions, an oily product was obtained,this was triturated with ether to give the title product as a white solid (0.126 g, 18%). NMR (300 MHz): 2.2 (s, 6H), 2.3–2.8 (m, 2H), 3.75–3.95 (m, 3H(, 4.82 (brs, 1H), 6.17 (d, 1H), 6.82 (d, 2H), 6.97 (t, 1H), 7.27 (t, 2H), 7.58 (d, 2H), 7.66 (d, 2H), 7.95 (d, 1H), 8.95 (s, 1H), 9.25 (s, 1H); m/z: (ES+) 380.4 (MH+).

후처리

  1. customwas partitioned between EtOAc and water
  2. washThe organic phase was washed with water
  3. dry with materialdried over MgSO4
  4. customevaporated at reduced pressure
  5. customThe residue was purified by chromatography (0.1%NH3 (aq), 3–10% MeOH in DCM as eluent)
  6. customUpon evaporation of the fractions
  7. customobtained,this was triturated with ether

출처 및 근거

ORD 기록
ord-13cbe94dd84b4283a8dfc0f879c51fc9
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07176212B2

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