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

HRID 2167850노트

반응식

HRID 2167850 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b8e37af2ebfe49bea1e889399c266e3a
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09045441B2

반응 노트

불러오는 중…