Triethylamine → HCID 178507669、化合物

HRID 1914841ノート

反応式

HRID 1914841 の反応式
[NH2:1]/[C:2](/OCC)=[CH:3]\[C:4](=O)[C:5]([F:8])([F:7])[F:6].Cl.[NH2:14][NH2:15].C(N(CC)CC)C>C(O)C>[F:6][C:5]([F:8])([F:7])[C:4]1[CH:3]=[C:2]([NH2:1])[NH:14][N:15]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 115031Hydrazinium chlorideHCID 151117544-Amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one

生成物 1

HCID 178507669HCID 178507669、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (E)-4-amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one, (Compound [XXIV]) (7.00 g, 38.2 mmol, 1.0 eq.) in ethanol (150 mL) in a 250 mL round bottom flask was added hydrazine hydrochloride (2.75 g, 40.16 mmol, 1.05 eq.) followed by triethylamine (4.05 g, 40.16 mmol, 1.05 eq.). The reaction mixture was heated to reflux for 16 hours. After cooling and concentration, the residue was purified by silica gel chromatography using CHCl3-MeOH (10%) as the eluant to give Compound [XXV]: LCMS m/e 152 (M+H); 1H NMR (400 MHz, DMSO-d6) δ ppm 5.32 (s, 2H) 5.51 (s, 1H) 12.12 (br. s., 1H).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 16 hours
  3. temperatureAfter cooling
  4. concentrationconcentration
  5. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-565f6522ba874b8aa693394e02a87fdf
出典データセット
uspto-grants-2013_12
特許番号
US08614221B2

反応ノート

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