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Methanol → N-[6-(1H-Indol-4-yl)-1-methyl-1H-indazol-4-yl]-2-pyridinecarboxamide

HRID 1616002
ノート
印刷プレビュー

反応式

HRID 1616002 の反応式
[NH:1]1[C:9]2[C:4](=[C:5]([C:10]3[CH:11]=[C:12]([NH2:20])[C:13]4[CH:14]=[N:15][N:16]([CH3:19])[C:17]=4[CH:18]=3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.CCN(C(C)C)C(C)C.Cl.[N:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[C:37](Cl)=[O:38].CO>C(Cl)Cl>[NH:1]1[C:9]2[C:4](=[C:5]([C:10]3[CH:18]=[C:17]4[C:13]([CH:14]=[N:15][N:16]4[CH3:19])=[C:12]([NH:20][C:37]([C:32]4[CH:33]=[CH:34][CH:35]=[CH:36][N:31]=4)=[O:38])[CH:11]=3)[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]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 887MethanolHCID 81531DiisopropylethylamineHCID 135033Picolinoyl Chloride HydrochlorideHCID 582680236-(1H-Indol-4-yl)-1-methyl-1H-indazol-4-amine

生成物 1

HCID 44540780N-[6-(1H-Indol-4-yl)-1-methyl-1H-indazol-4-yl]-2-pyridinecarboxamide収率 23.2%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

6-(1H-Indol-4-yl)-1-methyl-1H-indazol-4-amine (70 mg, 0.27 mmol) was dissolved in DCM (3 ml) and treated with DIPEA (0.145 ml). 2-Pyridinecarbonyl chloride hydrochloride (59.5 mg, 0.34 mmol) was added and the reaction was stirred for 5 h. MeOH (2 ml) was added and the reaction stirred overnight. The solvent was evaporated and the residue was treated with DCM/Methanol (1:1, 2 ml) then evaporated to dryness. The product was dissolved in DMSO (2 ml) and purified by Mass Directed Automated Preparative HPLC (Method B). Fractions containing product were combined and dried to give the title compound (23 mg).

後処理

  1. stirringthe reaction stirred overnight
  2. customThe solvent was evaporated
  3. additionthe residue was treated with DCM/Methanol (1:1, 2 ml)
  4. customthen evaporated to dryness
  5. dissolutionThe product was dissolved in DMSO (2 ml)
  6. custompurified by Mass Directed Automated Preparative HPLC (Method B)
  7. additionFractions containing product
  8. customdried

出典と根拠

ORDレコード
ord-3871c9899bb0483b8250bb552bb65e63
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765743B2

反応ノート

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