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Hydrazine hydrate (1:1) → HCID 66985760, 화합물

HRID 2064672
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반응식

HRID 2064672 반응식
[CH2:1]([O:3][C:4](=[O:17])[CH:5]([C:14](=O)[CH3:15])[C:6](=O)[CH2:7][O:8][C:9]([CH3:12])([CH3:11])[CH3:10])[CH3:2].O.[NH2:19][NH2:20]>C(O)(=O)C>[CH2:1]([O:3][C:4]([C:5]1[C:6]([CH2:7][O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[N:19][NH:20][C:14]=1[CH3:15])=[O:17])[CH3:2]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 85826160HCID 85826160, 화합물

생성물 1

HCID 66985760HCID 66985760, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 2-acetyl-4-tert-butoxy-3-oxo-butyric acid ethyl ester [0.325 g, Reference Example 46] in acetic acid (3 ml) was added hydrazine hydrate (71 μL). The mixture was stirred at ambient temperature for 16 hours and then evaporated to remove the acetic acid. The residue was dissolved in ethyl acetate and the solution was washed with 5% sodium hydrogen carbonate solution, then with water, then dried over magnesium sulfate, and then evaporated to yield 3-tert-butyloxymethyl-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (0.258 g) as a yellow oil which was used without further purification. LC-MS (METHOD B): RT=3.22 minutes; 241 (M+H)+.

후처리

  1. customevaporated
  2. customto remove the acetic acid
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washthe solution was washed with 5% sodium hydrogen carbonate solution
  5. dry with materialwith water, then dried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-8b2c63d953b44369808704f41c421ad3
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288425B2

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