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Butyl iodide → 5-Amino-2-butylpyrazol-3-carboxylic acid ethyl ester

HRID 1747266
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HRID 1747266 반응식
[H-].[Na+].[CH2:3]([O:5][C:6]([C:8]1[CH:12]=[C:11]([NH2:13])[NH:10][N:9]=1)=[O:7])[CH3:4].[CH2:14](I)[CH2:15][CH2:16][CH3:17]>C(#N)C>[CH2:3]([O:5][C:6]([C:8]1[N:9]([CH2:14][CH2:15][CH2:16][CH3:17])[N:10]=[C:11]([NH2:13])[CH:12]=1)=[O:7])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10962Butyl iodideHCID 24758Sodium hydrideHCID 178469278HCID 178469278, 화합물

생성물 1

HCID 196199605-Amino-2-butylpyrazol-3-carboxylic acid ethyl ester수율 38%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Sodium hydride (920 mg, 21 mmol) was added to a solution of 5-aminopyrazol-3-carboxylic acid ethyl ester (3.10 g, 20 mmol) in acetonitrile (100 mL) under a nitrogen atmosphere, and the obtained mixture was then stirred at room temperature for 30 minutes. The reaction solution was cooled on ice, and butyl iodide (2.3 mL, 20 mmol) was then added thereto. The obtained mixture was stirred at room temperature for 1 hour, and then at 60° C. for 1 hour. The reaction solution was left at room temperature overnight. Thereafter, the solvent was distilled away, and water was then added to the residue, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated saline, and it was dried over sodium sulfate and was then concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate), so as to obtain the title compound (1.60 g, yield: 38%) in the form of a pale yellow oily substance.

후처리

  1. additionwas then added
  2. stirringThe obtained mixture was stirred at room temperature for 1 hour
  3. waitat 60° C. for 1 hour
  4. waitThe reaction solution was left at room temperature overnight
  5. distillationThereafter, the solvent was distilled away
  6. additionwater was then added to the residue
  7. extractionfollowed by extraction with ethyl acetate
  8. washThe organic layer was washed with water
  9. dry with materiala saturated saline, and it was dried over sodium sulfate
  10. concentrationwas then concentrated
  11. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-e07b1ed8902c4ac7be00c210a512a217
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150563B2

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