Water → Pyrrolo[1,2-b]pyridazin-4(1H)-one

HRID 2117075ノート

反応式

HRID 2117075 の反応式
[O:1]=[C:2]1[C:7](C(OCC)=O)=[CH:6][NH:5][N:4]2[CH:13]=[CH:14][CH:15]=[C:3]12.[Na+].[Cl-].O>CS(C)=O>[NH:5]1[CH:6]=[CH:7][C:2](=[O:1])[C:3]2=[CH:15][CH:14]=[CH:13][N:4]12

参加物

5

反応物 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 10104421ETHYL 4-OXO-1,4-DIHYDROPYRROLO[1,2-B]PYRIDAZINE-3-CARBOXYLATE

生成物 1

HCID 57415871Pyrrolo[1,2-b]pyridazin-4(1H)-one収率 67.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

反応条件

温度
150 °C

実験手順

A mixture of ethyl 4-oxo-1,4-dihydropyrrolo[1,2-b]pyridazine-3-carboxylate (206 mg, 1.0 mmol), NaCl (64 mg, 1.1 mmol), water (0.054 mL, 3.0 mmol) and DMSO (2 mL) was heated at 150° C. for 3 hours. At the end of the reaction DMSO was distilled off and the residue was purified by silica gel flash chromatography (eluted with 1-10% EtOAc/CH2Cl2) to give the title compound (90 mg, 67%) as a light yellow solid.

後処理

  1. distillationwas distilled off
  2. customthe residue was purified by silica gel flash chromatography (eluted with 1-10% EtOAc/CH2Cl2)

出典と根拠

ORDレコード
ord-433b315bf8df484693d91ac2f49dc1fb
出典データセット
uspto-grants-2008_10
特許番号
US07439246B2

反応ノート

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