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Hydrazine hydrate (1:1) → Tert-butyl 4-cyano-5-hydrazinothiophene-2-carboxylate

HRID 1096152
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HRID 1096152 반응식
[C:1]([C:3]1[CH:4]=[C:5]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[S:6][C:7]=1S(C)(=O)=O)#[N:2].O.[NH2:20][NH2:21]>CO.C(OCC)(=O)C>[C:1]([C:3]1[CH:4]=[C:5]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[S:6][C:7]=1[NH:20][NH2:21])#[N:2]
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 66785761Tert-butyl 4-cyano-5-(methylsulfonyl)thiophene-2-carboxylate

생성물 1

HCID 11622817Tert-butyl 4-cyano-5-hydrazinothiophene-2-carboxylate

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

A mixture of tert-butyl 4-cyano-5-(methylsulfonyl)thiophene-2-carboxylate (2.0 g, 7.0 mmol) and hydrazine hydrate (1.7 mL) in methyl alcohol (30 mL) was stirred at 60° C. for 2 hours. The reaction mixture was diluted with ethyl acetate (100 mL) and washed with water. Organic layer was separated, dried over anhydrous sodium sulfate and evaporated. Through chromatography purification (n-hexane/ethyl acetate 3:2), 1 g of the title compound was thus obtained.

후처리

  1. washwashed with water
  2. customOrganic layer was separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated
  5. customThrough chromatography purification (n-hexane/ethyl acetate 3:2), 1 g of the title compound
  6. customwas thus obtained

출처 및 근거

ORD 기록
ord-d1c8815be73c441b93a2ef2e2ef60399
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08138217B2

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