Water → 2-(4-Bromo-phenyl)-thiomorpholin-3-one

HRID 2167850ノート

反応式

HRID 2167850 の反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].C([O-])([O-])=O.[K+].[K+].C([O:14][C:15](=O)[CH:16](Br)[C:17]1[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=1)C.O>CCO>[Br:23][C:20]1[CH:21]=[CH:22][C:17]([CH:16]2[S:5][CH2:4][CH2:3][NH:2][C:15]2=[O:14])=[CH:18][CH:19]=1

参加物

6

反応物 4

HCID 962WaterHCID 9082Cysteamine HydrochlorideHCID 11430Potassium CarbonateHCID 12754876Ethyl 2-bromo-(4-bromophenyl)acetate

生成物 1

HCID 666540542-(4-Bromo-phenyl)-thiomorpholin-3-one収率 77.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-aminoethanethiol hydrochloride (6.93 g; 61 mmol) in EtOH (400 mL) was added K2CO3 (16.86 g; 122 mmol), at RT, followed after 15 minutes by bromo-(4-bromo-phenyl)-acetic acid ethyl ester (12 mL; 61 mmol). The resulting mixture was stirred at RT for two days, subsequently, water was added and the resulting mixture was extracted with EtOAc. The combined organic layers were dried (MgSO4), filtered, and concentrated in vacuo. The residue was recrystallized from EtOH to afford 2-(4-bromo-phenyl)-thiomorpholin-3-one (12.8 g).

後処理

  1. extractionthe resulting mixture was extracted with EtOAc
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was recrystallized from EtOH

出典と根拠

ORDレコード
ord-b8e37af2ebfe49bea1e889399c266e3a
出典データセット
uspto-grants-2015_06
特許番号
US09045441B2

反応ノート

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