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Water → HCID 59639515, 화합물

HRID 2249743
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HRID 2249743 반응식
CS([C:5]1[N:6]=[C:7]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:8]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:9]=2[N:10]=1)(=O)=O.CN1C(=O)CCC1.[CH2:35]([N:37]([CH2:41][CH3:42])[CH2:38][CH2:39][NH2:40])[CH3:36].O>CCOC(C)=O>[CH2:35]([N:37]([CH2:41][CH3:42])[CH2:38][CH2:39][NH:40][C:5]1[N:6]=[C:7]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:8]2[CH:14]=[CH:13][C:12](=[O:15])[N:11]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:9]=2[N:10]=1)[CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 13387N-methyl-2-pyrrolidoneHCID 60993N,N-DiethylethylenediamineHCID 59639663HCID 59639663, 화합물

생성물 1

HCID 59639515HCID 59639515, 화합물수율 101.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of the product of Example 46 (18.8 mg, 0.05 mmol), NMP (5 mL) and N,N-diethylethylenediamine (28 mg, 0.25 mmol, 5 eq) was heated to 50°. After 1 h, H2O (20 mL) was added and then EtOAc (20 mL). The layers were separated. The organic layer was washed with satd aq NaCl, dried (MgSO4) filtered and the solvent was evaporated in vacuo. The yellow residue was purified by Flash chromatography to afford 2-(2-diethylamino-ethylamino)-4,8-diphenyl-8H-pyrido[2,3-d]pyrimidin-7-one (21 mg, 89% yield). 1H-NMR (CDCl3) δ 0.74-0.98 (m, 6H), 2.28-2.56 (m, 8H), 2.98 (br s, 1H), 6.32 (d, 1H, J=9.8 Hz), 7.26 (m, 2H), 7.09-7.88 (m, 1H), LC MS (m/e)=414 (MH+).

후처리

  1. customThe layers were separated
  2. washThe organic layer was washed with satd aq NaCl
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was evaporated in vacuo
  6. customThe yellow residue was purified by Flash chromatography

출처 및 근거

ORD 기록
ord-c4ee8b9d42344c1eb059d63953608cd7
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314881B2

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