Hydrochloric Acid → HCID 178460024、化合物

HRID 1349784ノート

反応式

HRID 1349784 の反応式
O1CCCCC1[N:7]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[N:20]=[CH:19][N:18](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:17]=3)=[CH:13][CH:14]=2)[C:9]([C:40]2[CH:41]=[C:42]([NH:46][C:47](=[O:56])[CH:48]([CH:50]3[CH2:55][CH2:54][CH2:53][NH:52][CH2:51]3)[CH3:49])[CH:43]=[CH:44][CH:45]=2)=[N:8]1.Cl.C([O-])(O)=O.[Na+]>O1CCOCC1>[NH:18]1[CH:19]=[N:20][C:16]([C:12]2[CH:11]=[C:10]3[C:15](=[CH:14][CH:13]=2)[NH:7][N:8]=[C:9]3[C:40]2[CH:41]=[C:42]([NH:46][C:47](=[O:56])[CH:48]([CH:50]3[CH2:55][CH2:54][CH2:53][NH:52][CH2:51]3)[CH3:49])[CH:43]=[CH:44][CH:45]=2)=[N:17]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 69423159N-(3-{1-Perhydro-2H-pyran-2-yl-5-[1-(triphenylmethyl)(1,2,4-triazol-3-yl)](1H-indazol-3-yl)}phenyl)-3-piperidylpropanamide

生成物 1

HCID 178460024HCID 178460024、化合物収率 38%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

N-(3-{1-Perhydro-2H-pyran-2-yl-5-[1-(triphenylmethyl)(1,2,4-triazol-3-yl)](1H-indazol-3-yl)}phenyl)-3-piperidylpropanamide was 4 mL of 4.0 N HCl in 1,4-dioxane. The reaction mixture was stirred at room temperature overnight. After neutralization with a saturated aqueous solution of NaHCO3, the crude reaction mixture was evaporated to dryness and purified by preparative HPLC (0.106 g, 38% yield over 2 steps): 1H NMR (CD3OD) δ 8.73 (br s, 1H), 8.35 (br s, 1H), 8.17 (t, 1H), 8.1 (dd, 1H), 7.7–7.6 (m, 3H), 7.5 (t, 1H), 2.8 (t, 2H), 2.66 (t, 2H), 2.58 (br s, 4H), 1.65 (m, 4H), 1.5 (m, 2H); ES-MS (m/z) 416 [M+H]+.

後処理

  1. customwas evaporated to dryness
  2. custompurified by preparative HPLC (0.106 g, 38% yield over 2 steps)

出典と根拠

ORDレコード
ord-11d02a477bd54fdcb3e95ccedae42aa7
出典データセット
uspto-grants-2007_05
特許番号
US07211594B2

反応ノート

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