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Potassium Iodide → HCID 58529656、化合物

HRID 1972713
ノート
印刷プレビュー

反応式

HRID 1972713 の反応式
[NH2:1][C:2]1[C:7]2=[CH:8][CH:9]=[C:10]([C:11](=[O:14])[CH2:12]Cl)[N:6]2[N:5]=[CH:4][N:3]=1.C([O-])([O-])=O.[K+].[K+].[I-].[K+].[CH2:23]([N:30]1[CH2:35][CH2:34][NH:33][CH:32]([CH2:36][O:37][Si:38]([C:41]([CH3:44])([CH3:43])[CH3:42])([CH3:40])[CH3:39])[CH2:31]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CN(C=O)C>[NH2:1][C:2]1[C:7]2=[CH:8][CH:9]=[C:10]([C:11](=[O:14])[CH2:12][N:33]3[CH2:34][CH2:35][N:30]([CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH2:31][CH:32]3[CH2:36][O:37][Si:38]([C:41]([CH3:44])([CH3:43])[CH3:42])([CH3:39])[CH3:40])[N:6]2[N:5]=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 585293111-{4-Aminopyrrolo[2,1-f][1,2,4]triazin-7-yl}-2-chloroethan-1-oneHCID 58529880HCID 58529880、化合物

生成物 1

HCID 58529656HCID 58529656、化合物収率 81%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 1-(4-aminopyrrolo[2,1-f][1,2,4]triazin-7-yl)-2-chloroethanone (1.00 g, 4.75 mmol), K2CO3 (1.97 g, 14.2 mmol) and potassium iodide (79 mg, 0.47 mmol) in DMF (20 mL), was added 1-benzyl-3-({[tert-butyl(dimethyl)silyl]oxy}methyl)piperazine (1.53 g, 4.79 mmol, prepared by the method of Naylor et al J. Med. Chem. 36, 2075). The reaction was allowed to stir for 17 hours. The mixture was partitioned between ethyl acetate (200 mL) and saturated, aqueous Na2CO3 solution (100 mL). The layers were separated and the organic was washed with brine, dried (Na2SO4), and evaporated. The crude material was purified by ISCO® chromatography using a gradient elution from 50% to 100% ethyl acetate in hexanes to obtain 1.9 g (81%) of the desired product LC-MS [M+H]+=495.6, RT=2.56 min.

後処理

  1. customprepared by the method of Naylor et al J
  2. customThe mixture was partitioned between ethyl acetate (200 mL)
  3. customThe layers were separated
  4. washthe organic was washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customThe crude material was purified by ISCO® chromatography
  8. washa gradient elution from 50% to 100% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-3b4125b3c1ed4951ab17abb723b4d053
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08431695B2

反応ノート

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