Formaldehyde → HCID 67981250, 화합물

HRID 1520026노트

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HRID 1520026 반응식
[CH2:1]=O.Cl.[N+:4]([C:7]1[CH:8]=[N:9][N:10]([CH:12]2[CH2:16][CH2:15][NH:14][CH2:13]2)[CH:11]=1)([O-:6])=[O:5]>C(O)=O>[CH3:1][N:14]1[CH2:15][CH2:16][CH:12]([N:10]2[CH:11]=[C:7]([N+:4]([O-:6])=[O:5])[CH:8]=[N:9]2)[CH2:13]1

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 67981150HCID 67981150, 화합물

생성물 1

HCID 67981250HCID 67981250, 화합물

시약·촉매·용매 1

HCID 284Formic Acid용매

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온도
100 °C

실험 절차

To a solution of Formic acid (50 ml) and Formaldehyde solution (50 mL) was added 4-Nitro-1-pyrrolidin-3-yl-1H-pyrazole hydrochloride (10 g). The reaction mixture was heated at 100° C. for 16 h. The reaction mixture was concentrated under reduced pressure. The residue was tarturated with acetonitrile (150 mL), filtered off solid and filtrate was concentrated. The crude material was basified with ammonia solution, extracted with ethyl acetate, dried over sodium sulphate and evaporated to afford (7 g, 78%) as pale yellow liquid. 1H NMR (400 Mz, DMSO-d6) δ 8.85 (s, 1H), 8.24 (s, 1H), 5.24 (m, 1H), 2.75-2.81 (m, 3H), 2.33-2.49 (m, 2H), 2.27 (s, 3H), 2.12 (m, 1H).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. filtrationfiltered off solid and filtrate
  3. concentrationwas concentrated
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over sodium sulphate
  6. customevaporated
  7. customto afford (7 g, 78%) as pale yellow liquid

출처 및 근거

ORD 기록
ord-a2fa40ec113641f986fb3ef5877c1fac
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073892B2

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