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

HRID 549426
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HRID 549426 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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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

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온도
60 °C
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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-c4469446dd5e4b05bf641b36dc639ed9
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943654B2

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