Formaldehyde → HCID 67981250、化合物

HRID 1520026ノート

反応式

HRID 1520026 の反応式
[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

参加物

4

反応物 2

HCID 712FormaldehydeHCID 67981150HCID 67981150、化合物

生成物 1

HCID 67981250HCID 67981250、化合物

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a2fa40ec113641f986fb3ef5877c1fac
出典データセット
uspto-grants-2015_07
特許番号
US09073892B2

反応ノート

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