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Diisopropylethylamine → HCID 178463538, 화합물

HRID 1192535
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HRID 1192535 반응식
Br[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][NH:6]2.[Si:11]([O:18][CH:19]1[CH2:24][CH2:23][N:22]([C:25]2[C:26]([CH:36]([NH2:38])[CH3:37])=[CH:27][C:28]([Cl:35])=[C:29]3[C:34]=2[N:33]=[CH:32][CH:31]=[CH:30]3)[CH2:21][CH2:20]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])[CH3:12].C(N(CC)C(C)C)(C)C>C(O)C>[Si:11]([O:18][CH:19]1[CH2:20][CH2:21][N:22]([C:25]2[C:26]([CH:36]([NH:38][C:2]3[N:10]=[CH:9][N:8]=[C:7]4[C:3]=3[N:4]=[CH:5][NH:6]4)[CH3:37])=[CH:27][C:28]([Cl:35])=[C:29]3[C:34]=2[N:33]=[CH:32][CH:31]=[CH:30]3)[CH2:23][CH2:24]1)([C:14]([CH3:17])([CH3:15])[CH3:16])([CH3:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 583685251-[8-(4-{[tert-Butyl(dimethyl)silyl]oxy}piperidin-1-yl)-5-chloroquinolin-7-yl]ethanamineHCID 178419477HCID 178419477, 화합물

생성물 1

HCID 178463538HCID 178463538, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 6-bromo-9H-purine (0.262 g, 1.31 mmol), 1-[8-(4-{[tert-butyl(dimethyl)silyl]oxy}piperidin-1-yl)-5-chloroquinolin-7-yl]ethanamine (0.276 g, 0.657 mmol), and N,N-diisopropylethylamine (0.23 mL, 1.31 mmol) in ethanol (2 mL) was heated at reflux under nitrogen overnight. The mixture was evaporated and the resulting residue was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried and evaporated to dryness. The crude product was used directly in the next step (0.20 g, 57%). LCMS calculated for C27H37ClN7OSi (M+H)+: m/z=538.2; Found: 538.2.

후처리

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen overnight
  3. customThe mixture was evaporated
  4. additionthe resulting residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. washThe combined organic layers were washed with brine
  7. customdried
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-8c991c9dd5bd4089b19ffde76c3fc9e5
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680108B2

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