Lawesson's reagent → 1-(Pyridazin-3-yl)ethan-1-ol

HRID 1503425ノート

反応式

HRID 1503425 の反応式
CON(C)[C:4]([C:6]1[N:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5].[CH3:13]OC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=S)=CC=1>O1CCOCC1>[N:8]1[CH:9]=[CH:10][CH:11]=[C:6]([CH:4]([OH:5])[CH3:13])[N:7]=1

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 58197546N-methoxy-N-methylpyridazine-3-carboxamide

生成物 1

HCID 151975111-(Pyridazin-3-yl)ethan-1-ol収率 328.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
150 °C

実験手順

A suspension of compound 2 (20 mg, 0.049 mmol) and Lawesson's Reagent (20 mg, 0.049 mmol) in anhydrous dioxane (1 mL) was stirred at 150° C. for 35 min in a CEM microware reactor. The mixture was concentrated in vacuo, and the residue was purified by prep-TLC to give compound 3 (20 mg, 96%) as a yellow solid.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by prep-TLC

出典と根拠

ORDレコード
ord-dbf595255c244f78b794729502c7168d
出典データセット
uspto-grants-2015_12
特許番号
US09212153B2

反応ノート

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