Hydrogen Bromide → 3-Methylpiperidin-4-one hydrobromide

HRID 249426ノート

反応式

HRID 249426 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-b7eb54ab6e2c4a5eb4df150132db8cb4
出典データセット
uspto-grants-1993_05
特許番号
US05214148

反応ノート

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