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Ammonium Chloride → Tert-butyl cis-2-(6-chloro-3-fluoro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate

HRID 1620035
ノート
印刷プレビュー

反応式

HRID 1620035 の反応式
[C:1]([NH2:10])([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)([CH3:3])[CH3:2].CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[C:33]([O:37][C:38]([NH:40][C@H:41]1[CH2:46][CH2:45][CH2:44][CH2:43][C@H:42]1[NH:47][C:48]1[C:56]([F:57])=[CH:55][C:51]([C:52](O)=[O:53])=[C:50]([Cl:58])[N:49]=1)=[O:39])([CH3:36])([CH3:35])[CH3:34].[Cl-].[NH4+]>C(OCC)(=O)C.CN(C=O)C.O>[Cl:58][C:50]1[N:49]=[C:48]([NH:47][C@H:42]2[CH2:43][CH2:44][CH2:45][CH2:46][C@H:41]2[NH:40][C:38](=[O:39])[O:37][C:33]([CH3:36])([CH3:34])[CH3:35])[C:56]([F:57])=[CH:55][C:51]=1[C:52]([NH:10][C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)([CH3:3])[CH3:2])=[O:53]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 25517Ammonium ChlorideHCID 68509CumylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 866838426-(cis-2-(Tert-butoxycarbonylamino)cyclohexylamino)-2-chloro-5-fluoronicotinic acid

生成物 1

HCID 86683841
Tert-butyl cis-2-(6-chloro-3-fluoro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Cumylamine (1.97 ml), WSC.HCl (2.62 g), and HOBt.H2O (2.10 g) were added to a DMF (60 ml) solution containing 6-(cis-2-(tert-butoxycarbonylamino)cyclohexylamino)-2-chloro-5-fluoronicotinic acid obtained in the 1st step, followed by stirring at room temperature for 4 hours. A saturated aqueous ammonium chloride solution and ethyl acetate were added to the reaction mixture. The organic layer was collected, washed with a saturated aqueous sodium hydrogen carbonate solution and then with saturated saline, and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. Diisopropylether and hexane were added to the obtained residue, solid matter was collected by filtration, and a white solid of tert-butyl cis-2-(6-chloro-3-fluoro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate (4.41 g) was thus obtained.

後処理

  1. customobtained in the 1st step
  2. customThe organic layer was collected
  3. washwashed with a saturated aqueous sodium hydrogen carbonate solution
  4. dry with materialwith saturated saline, and dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. additionDiisopropylether and hexane were added to the obtained residue, solid matter
  7. filtrationwas collected by filtration

出典と根拠

ORDレコード
ord-fa21bf6621e946d38a9d8249b8271fb6
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772320B2

反応ノート

読み込み中…

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