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Sodium Iodide → Formic acid 2-[(4,4-dimethyl-1-piperidinyl)methyl]-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-1,3-thiazole-4-carboxamide

HRID 244752
ノート
印刷プレビュー

反応式

HRID 244752 の反応式
Cl[CH2:2][C:3]1[S:4][CH:5]=[C:6]([C:8]([NH:10][C:11]2[CH:19]=[C:18]([C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[CH:17]=[C:16]3[C:12]=2[CH:13]=[N:14][N:15]3S(C2C=CC=CC=2)(=O)=O)=[O:9])[N:7]=1.Cl.[CH3:39][C:40]1([CH3:46])[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1.CCN(C(C)C)C(C)C.[I-].[Na+].C[Si](C)(C)[O-:60].[K+]>C(#N)C.C1COCC1>[CH:8]([OH:9])=[O:60].[CH3:39][C:40]1([CH3:46])[CH2:45][CH2:44][N:43]([CH2:2][C:3]2[S:4][CH:5]=[C:6]([C:8]([NH:10][C:11]3[CH:19]=[C:18]([C:20]4[CH:28]=[CH:27][CH:26]=[C:25]5[C:21]=4[CH:22]=[CH:23][NH:24]5)[CH:17]=[C:16]4[C:12]=3[CH:13]=[N:14][NH:15]4)=[O:9])[N:7]=2)[CH2:42][CH2:41]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 5238Sodium IodideHCID 81531DiisopropylethylamineHCID 222529024,4-Dimethylpiperidinium chlorideHCID 23668039Potassium trimethylsilanolate2 回HCID 583563582-(Chloromethyl)-N-[6-(1H-indol-4-yl)-1-(phenylsulfonyl)-1H-indazol-4-yl]-1,3-thiazole-4-carboxamide

生成物 1

HCID 67319980
Formic acid 2-[(4,4-dimethyl-1-piperidinyl)methyl]-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-1,3-thiazole-4-carboxamide
収率 26.4%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
70 °C

実験手順

A solution of 2-(chloromethyl)-N-[6-(1H-indol-4-yl)-1-(phenylsulfonyl)-1H-indazol-4-yl]-1,3-thiazole-4-carboxamide (55 mg, 0.1 mmol) in acetonitrile (0.5 ml) was added to 4,4-dimethylpiperidine hydrochloride (0.11 mmol, available from Microchemistry Ltd). DIPEA was then added (0.026 ml, 0.15 mmol), followed by sodium iodide (13 mg). The vial was capped and the stirred solution heated to 70° C. for 18 h. Potassium trimethylsilanolate (26 mg) was dissolved in THF (0.3 ml) and added to the vessel, which was then stirred at room temperature for 21 h, then heated at 50° C. for 3 h. A further equivalent of potassium trimethylsilanolate was added as a solution in THF (150 ul) and the mixture was heated at 50° C. for a further 18 h. The solution was quenched with aqueous acetonitrile (500 ul, 50:50) and neutralised. Solvent was removed by blowdown. The residue was dissolved in DMSO 0.5 mL and purified by Mass Directed AutoPrep HPLC (Method F). The solvent was removed by vacuum centrifugation to give the title compound (7 mg). LCMS (Method C) Rt=1.69 min, MH+=485.

後処理

  1. customThe vial was capped
  2. additionadded to the vessel, which
  3. temperatureheated at 50° C. for 3 h
  4. temperaturethe mixture was heated at 50° C. for a further 18 h
  5. customThe solution was quenched with aqueous acetonitrile (500 ul, 50:50)
  6. customSolvent was removed by blowdown
  7. dissolutionThe residue was dissolved in DMSO 0.5 mL
  8. custompurified by Mass Directed AutoPrep HPLC (Method F)
  9. customThe solvent was removed by vacuum centrifugation

出典と根拠

ORDレコード
ord-24efc96a350d40c3a9b5ea4bc42e133c
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658635B2

反応ノート

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