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Tetrahydrofuran → Ethyl 4-[1-[(10-(methoxymethyl)-10H-pyrazino[2,3-b][1,4]benzothiazin-8-ylmethyl]carbamoyl]piperidin-4-yl]-2-methylbutanoate

HRID 1059364
ノート
印刷プレビュー

反応式

HRID 1059364 の反応式
[N:1]1[C:10]2[NH:9][C:8]3[CH:11]=[C:12]([CH2:15]C(O)=O)[CH:13]=[CH:14][C:7]=3[S:6][C:5]=2[N:4]=[CH:3][CH:2]=1.C([N:21]([CH2:24]C)CC)C.[N-]=[N+]=[N-].P([O-])(OC1C=CC=CC=1)(OC1C=CC=CC=1)=[O:30].[NH:46]1[CH2:51][CH2:50][CH:49]([CH2:52][CH2:53][CH:54]([CH3:60])[C:55]([O:57][CH2:58][CH3:59])=[O:56])[CH2:48][CH2:47]1.[O:61]1[CH2:65]CC[CH2:62]1>C(OCC)(=O)C>[CH3:62][O:61][CH2:65][N:9]1[C:8]2[CH:11]=[C:12]([CH2:15][NH:21][C:24]([N:46]3[CH2:51][CH2:50][CH:49]([CH2:52][CH2:53][CH:54]([CH3:60])[C:55]([O:57][CH2:58][CH3:59])=[O:56])[CH2:48][CH2:47]3)=[O:30])[CH:13]=[CH:14][C:7]=2[S:6][C:5]2[N:4]=[CH:3][CH:2]=[N:1][C:10]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 11298836Ethyl 4-(piperidin-4-yl)-2-methylbutanoateHCID 1867013310H-Pyrazino[2,3-b][1,4]benzothiazine-8-acetic acidHCID 21964642Diphenylphosphate azide

生成物 1

HCID 18670562
Ethyl 4-[1-[(10-(methoxymethyl)-10H-pyrazino[2,3-b][1,4]benzothiazin-8-ylmethyl]carbamoyl]piperidin-4-yl]-2-methylbutanoate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 0.7 g of 10H-pyrazino[2,3-b][1,4]benzothiazine-8-acetic acid in tetrahydrofuran (50 ml) were added 0.35 ml of triethylamine and 0.55 ml of diphenyl phosphate azide and the resulting mixture was stirred at room temperature for 3 hours. Next, it was heated under reflux for 1.5 hours. After adding 0.55 g of ethyl 4-(piperidin-4-yl)-2-methylbutanoate, the resulting mixture was reacted at room temperature for 1 hour. After adding ethyl acetate, the reaction mixture was washed with water and dried over anhydrous magnesium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 0.66 g of the title compound as a yellow oily substance.

後処理

  1. temperatureNext, it was heated
  2. temperatureunder reflux for 1.5 hours
  3. customthe resulting mixture was reacted at room temperature for 1 hour
  4. washthe reaction mixture was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationAfter distilling off the solvent under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

出典と根拠

ORDレコード
ord-e7bbc59923dd46089f7334316f7b69c9
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06518423B1

反応ノート

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