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N,N-Dimethylethylenediamine → Ammonium Hydroxide

HRID 223001
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HRID 223001 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16](S(C)(=O)=O)[N:17]=[C:18]([C:19]3[CH:20]=[C:21]([CH:28]=[CH:29][C:30]=3[CH3:31])[C:22]([NH:24][CH2:25][CH2:26][CH3:27])=[O:23])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36].[CH3:37][N:38]([CH3:42])[CH2:39][CH2:40][NH2:41]>C(Cl)Cl>[NH4+:9].[OH-:23].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[N:9]1[C:14]2[N:15]=[C:16]([NH:41][CH2:40][CH2:39][N:38]([CH3:42])[CH3:37])[N:17]=[C:18]([C:19]3[CH:20]=[C:21]([CH:28]=[CH:29][C:30]=3[CH3:31])[C:22]([NH:24][CH2:25][CH2:26][CH3:27])=[O:23])[C:13]=2[CH:12]=[CH:11][C:10]1=[O:36]
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참가 물질

5

반응물 2

HCID 66053N,N-DimethylethylenediamineHCID 592126843-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide

생성물 2

HCID 14923Ammonium HydroxideHCID 592127323-(8-(2,6-difluorophenyl)-2-{[2-(dimethylamino)ethyl]amino}-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl)-4-methyl-N-propylbenzamide

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (0.07 g, 0.13 mmol), N,N-dimethylethylenediamine (0.0173 g, 0.15 mmol), and TEA (0.026 g, 0.26 mmol) were combined in CH2Cl2 (5 mL) and stirred under argon at room temperature for 1 h. The solvents were pumped off in vacuo. The residue was flash chromatographed on silica gel (10 g) eluted with CH2Cl2 to 6:1:0.1, CH2Cl2:ethanol:NH4OH to give the title compound as a white amorphous solid. mp 139-142° C. LC-MS m/z 521 (M+H)+, 1.61 min (ret time).

후처리

  1. customchromatographed on silica gel (10 g)
  2. washeluted with CH2Cl2 to 6:1:0.1, CH2Cl2

출처 및 근거

ORD 기록
ord-8d8c2030dc334f8182b0ee96102ad846
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08207176B2

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