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Dimethylformamide → 4-[3-((2S,6R)-2,6-Dimethyl-piperidin-1-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yloxy]-cyclohexylamine

HRID 2200046
ノート
印刷プレビュー

反応式

HRID 2200046 の反応式
[H-].[Na+].[NH2:3][C@H:4]1[CH2:9][CH2:8][C@H:7]([OH:10])[CH2:6][CH2:5]1.F[C:12]1[CH:13]=[CH:14][C:15]2[N:16]([C:18]([N:21]3[CH2:26][CH2:25][CH2:24][CH2:23][C@@H:22]3[CH3:27])=[N:19][N:20]=2)[CH:17]=1.[CH3:28]N(C=O)C>>[CH3:27][C@H:22]1[CH2:23][CH2:24][CH2:25][C@@H:26]([CH3:28])[N:21]1[C:18]1[N:16]2[CH:17]=[C:12]([O:10][CH:7]3[CH2:8][CH2:9][CH:4]([NH2:3])[CH2:5][CH2:6]3)[CH:13]=[CH:14][C:15]2=[N:20][N:19]=1
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 4

HCID 6228Dimethylformamide2 回HCID 24758Sodium hydrideHCID 866871056-Fluoro-3-((S)-2-methyl-piperidin-1-yl)-[1,2,4]triazolo[4,3-a]pyridineHCID 178511715HCID 178511715、化合物

生成物 1

HCID 1177290354-[3-((2S,6R)-2,6-Dimethyl-piperidin-1-yl)-[1,2,4]triazolo[4,3-a]pyridin-6-yloxy]-cyclohexylamine収率 27%

実験手順

Sodium hydride (60% in mineral oil, 0.26 g, 6.39 mmol) was added to a stirred solution of trans-4-amino cyclohexanol (0.397 g, 3.45 mmol) in anhydrous DMF (10 mL) at RT under an argon atmosphere. The reaction mixture was stirred at RT for 30 min, then Intermediate 2d (0.50 g, 2.13 mmol) in anhydrous DMF (4 mL) was added and stirred at 60° C. for 10 h. After cooling, the reaction mixture was quenched by careful addition of a saturated aqueous solution of NH4Cl and water (1:1) and extracted with EtOAc and then DCM. The combined organic extracts were concentrated in vacuo and the resultant residue was purified by FCC, using 0-25% [2M NH3 in MeOH] in DCM, to afford the title compound (0.193 g, 27%) as an orange residue. LCMS (Method 3): Rt 2.00 min, m/z 330 [MH+].

後処理

  1. stirringstirred at 60° C. for 10 h
  2. temperatureAfter cooling
  3. customthe reaction mixture was quenched by careful addition of a saturated aqueous solution of NH4Cl and water (1:1)
  4. extractionextracted with EtOAc
  5. concentrationThe combined organic extracts were concentrated in vacuo
  6. customthe resultant residue was purified by FCC

出典と根拠

ORDレコード
ord-2b30c960f306467ebcbbe8bf7635586b
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09359354B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート