Hydrogen Bromide → 3-Methylpiperidin-4-one hydrobromide

HRID 654128ノート

反応式

HRID 654128 の反応式
C([N:5]1[CH2:10][CH2:9][C:8](=[O:11])[C:7](C(OC)=O)([CH3:12])[CH2:6]1)(OC)=O.[BrH:17]>CO>[BrH:17].[CH3:12][CH:7]1[C:8](=[O:11])[CH2:9][CH2:10][NH:5][CH2:6]1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 3015585Dimethyl 3-methyl-4-oxopiperidine-1,3-dicarboxylate

生成物 1

HCID 200945873-Methylpiperidin-4-one hydrobromide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1,3-dicarbomethoxy-3-methyl-4-piperidone (51.45 g, 225 mmol) in hydrobromic acid (48%, 250 mL) is heated under reflux for 4 h and then cooled to room temperature. The resultant solution is concentrated in vacuo to give an orange colored solid. The solid is suspended in methanol (50 mL) and concentrated in vacuo again to give 3-methyl-4-piperidone hydrobromide salt: 42.9 g; 98%; mp 203°-205° C.

後処理

  1. temperatureunder reflux for 4 h
  2. concentrationThe resultant solution is concentrated in vacuo
  3. customto give an orange colored solid
  4. concentrationconcentrated in vacuo again

出典と根拠

ORDレコード
ord-f93e8ecb4d8445cd8f7ec67a6d88decd
出典データセット
uspto-grants-1992_07
特許番号
US05130321

反応ノート

読み込み中…