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Methylhydrazine → HCID 18436984, 화합물

HRID 456556
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HRID 456556 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([C:16]2[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][C:17]=2F)=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:27][NH:28][NH2:29].C([O-])(O)=O.[Na+]>C(O)CCC>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[C:16]3[C:17](=[CH:18][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:20][CH:21]=3)[N:28]([CH3:27])[N:29]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6061MethylhydrazineHCID 516892Sodium BicarbonateHCID 23112486HCID 23112486, 화합물

생성물 1

HCID 18436984HCID 18436984, 화합물수율 82.4%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A solution of (1-benzyl-piperidin-4-yl)-(2-fluoro-4-trifluoromethyl-phenyl)-methanone (2.0 g, 5.46 mmol), methylhydrazine (327 mg, 7.10 mmol), and n-butanol (22 mL) was heated at 120° C. in a seal vessel for 18 hours. The reaction was cooled to room temperature and basified with NaHCO3 and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (50 mL), dried over magnesium sulfate, filtered, and evaporated. The product was chromatographed on silica, eluting with 1:1 ethyl acetate/heptane, to afford 1.68 g (82%) of the desired product as an oil.

후처리

  1. extractionextracted with EtOAc (3×50 mL)
  2. washThe combined organic layers were washed with brine (50 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe product was chromatographed on silica
  7. washeluting with 1:1 ethyl acetate/heptane

출처 및 근거

ORD 기록
ord-c194978210424f2dadf6fda462ae7895
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07186724B2

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