Ammonium Sulfate → 4,4-Dimethylpyrrolidine-2-carboxylic acid

HRID 1158896ノート

反応式

HRID 1158896 の反応式
Cl[CH:2]1[CH2:7][C:6]([CH3:9])([CH3:8])[CH2:5][NH:4][C:3]1=[O:10].S([O-])([O-])(=O)=[O:12].[NH4+].[NH4+]>O>[CH3:9][C:6]1([CH3:8])[CH2:5][NH:4][CH:2]([C:3]([OH:10])=[O:12])[CH2:7]1

参加物

4

反応物 2

HCID 6097028Ammonium SulfateHCID 219413793-Chloro-5,5-dimethylpiperidin-2-one

生成物 1

HCID 2866424,4-Dimethylpyrrolidine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A suspension of 20.4 g (0.13 mol) of 3-chloro-5,5-dimethyl-2-piperidone and 45.2 g (0.14 mol) of Ba(OH)3-8H2O in 252 mL of water was heated in a Parr apparatus at 150° C. for 6 h. Then, 18.6 g (0.14 mol) of ammonium sulphate were added. The precipitate was filtered off, and the solution was concentrated under reduced pressure to dryness. Crude 4,4-dimethylpyrrolidine-2-carboxylic acid was obtained as a white solid (37.5 g). (J. Med. Chem., 20, 1176 (1977), EP 0 447 704 A1, page 17)

後処理

  1. filtrationThe precipitate was filtered off
  2. concentrationthe solution was concentrated under reduced pressure to dryness

出典と根拠

ORDレコード
ord-dfb2748e8a90434eb618196b1d014880
出典データセット
uspto-grants-2010_10
特許番号
US07812014B2

反応ノート

読み込み中…