Ethanolamine → 2-Chloro-6-(2-hydroxyethyl)-6,7-dihydro-5H-pyrrolo[3,4-b]pyridin-5-one

HRID 1799545ノート

反応式

HRID 1799545 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([CH2:8]Cl)[C:5]([C:10]([O:12]C)=O)=[CH:4][CH:3]=1.[CH2:14]([CH2:16][NH2:17])[OH:15]>CO>[Cl:1][C:2]1[N:7]=[C:6]2[CH2:8][N:17]([CH2:16][CH2:14][OH:15])[C:10](=[O:12])[C:5]2=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 700Ethanolamine3 回HCID 59525762Methyl 6-chloro-2-(chloromethyl)pyridine-3-carboxylate

生成物 1

HCID 582166462-Chloro-6-(2-hydroxyethyl)-6,7-dihydro-5H-pyrrolo[3,4-b]pyridin-5-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl 6-chloro-2-(chloromethyl)pyridine-3-carboxylate (0.1 g, 0.45 mmol) and ethanolamine (0.11 mL, 1.82 mmol) were stirred in MeOH (10 mL) at room temperature overnight. Additional ethanolamine (0.11 mL, 1.82 mmol) was added and stirring continued for 8 hours. Additional ethanolamine (0.22 mL, 3.64 mmol) was then added and stirring continued for 3 days. The solvent was removed in vacuo and the residue purified by silica gel chromatography (0-5% MeOH/EtOAc) to give the title compound as a white solid.

後処理

  1. stirringstirring
  2. waitcontinued for 3 days
  3. customThe solvent was removed in vacuo
  4. customthe residue purified by silica gel chromatography (0-5% MeOH/EtOAc)

出典と根拠

ORDレコード
ord-87509003de184f31a930ef55e7722664
出典データセット
uspto-grants-2013_01
特許番号
US08344144B2

反応ノート

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