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Trifluoroacetic acid → 6-(cis-2-Aminocyclohexylamino)-5-chloro-2-(5-methylpyridin-3-ylamino)nicotinamide.hydrochloride

HRID 2406771
ノート
印刷プレビュー

反応式

HRID 2406771 の反応式
[Cl:1][C:2]1[C:3]([NH:28][C@H:29]2[CH2:34][CH2:33][CH2:32][CH2:31][C@H:30]2[NH:35]C(=O)OC(C)(C)C)=[N:4][C:5]([NH:20][C:21]2[CH:22]=[N:23][CH:24]=[C:25]([CH3:27])[CH:26]=2)=[C:6]([C:8]([NH:10]C(C2C=CC=CC=2)(C)C)=[O:9])[CH:7]=1.C(O)(C(F)(F)F)=O>>[NH2:35][C@H:30]1[CH2:31][CH2:32][CH2:33][CH2:34][C@H:29]1[NH:28][C:3]1[C:2]([Cl:1])=[CH:7][C:6]([C:8]([NH2:10])=[O:9])=[C:5]([NH:20][C:21]2[CH:22]=[N:23][CH:24]=[C:25]([CH3:27])[CH:26]=2)[N:4]=1.[ClH:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 86683894Tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate

生成物 1

HCID 867625046-(cis-2-Aminocyclohexylamino)-5-chloro-2-(5-methylpyridin-3-ylamino)nicotinamide.hydrochloride収率 192.3%

実験手順

A mixture of tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate (12 mg) and TFA (0.5 ml) was stirred at room temperature for 1 hour. The solvent was distilled away under reduced pressure (at 40° C. or less), ethyl acetate and 4N hydrogen chloride/1,4-dioxane (25 μl) were added, and the resultant was left at rest overnight at room temperature. Solid matter was collected by filtration, and a white solid of 6-(cis-2-aminocyclohexylamino)-5-chloro-2-(5-methylpyridin-3-ylamino)nicotinamide•hydrochloride (8 mg) was thus obtained.

後処理

  1. distillationThe solvent was distilled away under reduced pressure (at 40° C. or less), ethyl acetate and 4N hydrogen chloride/1,4-dioxane (25 μl)
  2. additionwere added
  3. waitthe resultant was left at rest overnight at room temperature
  4. filtrationSolid matter was collected by filtration

出典と根拠

ORDレコード
ord-dcc6aefa5abb47d18fd0b244cc2681a6
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809371B2

反応ノート

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