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Sodium Hydroxide → 2-Bromo-2-methyl-1-(4-piperidinophenyl)-propan-1-one

HRID 981754
ノート
印刷プレビュー

反応式

HRID 981754 の反応式
[CH3:1][CH:2]([CH3:17])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1)=[O:4].ClS(O)(=O)=O.[Br:23]Br.[OH-].[Na+]>C(O)(=O)C>[Br:23][C:2]([CH3:17])([CH3:1])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 24408BromineHCID 24638Chlorosulfonic acidHCID 212571912-Methyl-1-(4-(piperidin-1-yl)phenyl)propan-1-one

生成物 1

HCID 198795192-Bromo-2-methyl-1-(4-piperidinophenyl)-propan-1-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

34.70 g (0.15 mol) of 2-methyl-1-(4-piperidinophenyl)-propan-1-one are dissolved in 200 ml of glacial acetic acid. 0.58 g (5.0 mmol) of chlorosulfonic acid (corresponding to 0.33 ml) are added as catalyst. 24.0 g (0.15 mol) of bromine are then added dropwise at room temperature with thorough stirring in the course of approximately one hour. The solution is then poured onto ice and is brought to about pH 6 with dilute sodium hydroxide solution. The precipitated crystals are extracted with toluene. The toluene solution is dried with Na2SO4 and is concentrated at 40° C. under the vacuum of a rotary evaporator. The slowly crystallising, orange liquid is then reacted further.

後処理

  1. additionThe solution is then poured onto ice
  2. extractionThe precipitated crystals are extracted with toluene
  3. dry with materialThe toluene solution is dried with Na2SO4
  4. concentrationis concentrated at 40° C. under the vacuum of a rotary evaporator
  5. customThe slowly crystallising
  6. customorange liquid is then reacted further

出典と根拠

ORDレコード
ord-c6c58e1d63984fa6918fa1968c1987af
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992547

反応ノート

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