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N-Pentylhydrazine → HCID 76629633, 화합물

HRID 2077265
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HRID 2077265 반응식
[CH2:1]([O:3][C:4](=[O:7])[CH:5]=O)[CH3:2].[CH2:8]([NH:13][NH2:14])[CH2:9][CH2:10][CH2:11][CH3:12]>C(O)C>[CH2:1]([O:3][C:4](=[O:7])[CH:5]=[N:14][NH:13][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH3:2]
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참가 물질

4

반응물 2

HCID 14247N-PentylhydrazineHCID 70211Ethyl oxoacetate

생성물 1

HCID 76629633HCID 76629633, 화합물수율 97.7%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To a magnetically stirred solution of oxo-acetic acid ethyl ester (35.08 ml, 177 mmol; 50% solution in toluene) in ethanol (450 ml) was added n-pentylhydrazine (21.7 g, 212 mmol) and the resulting solution was heated at 80° C. for 16 hours. The obtained mixture was allowed to attain room temperature and concentrated. The resulting residue was taken up in ethylacetate and water. The organic layer was separated and subsequently dried over MgSO4, filtered and concentrated to give (pentylhydrazono)acetic acid ethyl ester (Intermediate II-1) (32.2 gram, 93% yield) as a purple colored oil. 1H-NMR (400 MHz, CDCl3) δ 0.87-0.94 (m, 3H), 1.25-1.42 (m, 7H), 1.55-1.68 (m, 2H), 3.17-3.23 (m, 1H), 3.35-3.45 (m, 1H), 4.28 (q, J=7, 2H), 6.51 (br s, 1H), 6.72 (s, 1H).

후처리

  1. customto attain room temperature
  2. concentrationconcentrated
  3. customThe organic layer was separated
  4. dry with materialsubsequently dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3902c89133f54e07afd1a99e5611efde
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928134B2

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