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Potassium tert-butoxide → HCID 178499450、化合物

HRID 1852482
ノート
印刷プレビュー

反応式

HRID 1852482 の反応式
[C:1]([C:4]1[C:5]([NH:25][C:26]2[CH:31]=[CH:30][C:29]([CH2:32][C:33]([O:35][CH3:36])=[O:34])=[CH:28][CH:27]=2)=[N:6][N:7](C2(CC#N)CCN(C(OC(C)(C)C)=O)CC2)[CH:8]=1)(=[O:3])[NH2:2].CC([O-])(C)C.[K+]>C1COCC1.[NH4+].[Cl-]>[C:1]([C:4]1[C:5]([NH:25][C:26]2[CH:27]=[CH:28][C:29]([CH2:32][C:33]([O:35][CH3:36])=[O:34])=[CH:30][CH:31]=2)=[N:6][NH:7][CH:8]=1)(=[O:3])[NH2:2]
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

5

反応物 2

HCID 23665647Potassium tert-butoxideHCID 86729389tert-butyl 4-(4-carbamoyl-3-{[4-(2-methoxy-2-oxoethyl)phenyl]amino}-1H-pyrazol-1-yl)-4-(cyanomethyl)piperidine-1-carboxylate

生成物 1

HCID 178499450HCID 178499450、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 25517Ammonium Chloride溶媒

反応条件

温度
0 °C

実験手順

To a solution of tert-Butyl 4-(4-carbamoyl-3-{[4-(2-methoxy-2-oxoethyl)phenyl]amino}-1H-pyrazol-1-yl)-4-(cyanomethyl)piperidine-1-carboxylate (226 mg, 0.46 mmol) in THF (2.3 mL) at 0° C. was added KOtBu (0.68 mL, 0.68 mmol, 1.0M in THF), and the mixture was stirred at 0° C. for 20 minutes, then ambient temperature for 20 minutes. The mixture was diluted with saturated aqueous NH4Cl, and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous MgSO4, and concentrated in vacuo. Et2O (5 mL) was added to the resulting oily residue and a solid precipitated out. This solid was collected by decant, and washed with Et2O to afford the title compound. LRMS (ESI) calc'd for C13H15N4O3 [M+H]+: 275. Found: 275.

後処理

  1. waitambient temperature for 20 minutes
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationconcentrated in vacuo
  6. additionEt2O (5 mL) was added to the resulting oily residue
  7. customa solid precipitated out
  8. customThis solid was collected
  9. customby decant
  10. washwashed with Et2O

出典と根拠

ORDレコード
ord-8ed422a1a7504791a16650a0c06fc589
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962608B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート