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Diisopropylethylamine → HCID 178463538、化合物

HRID 1192535
ノート
印刷プレビュー

反応式

HRID 1192535 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 178463538HCID 178463538、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c991c9dd5bd4089b19ffde76c3fc9e5
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680108B2

反応ノート

読み込み中…

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