Acetic Acid → 6,7,8,9-Tetrahydro-3-hydroxy-2-phenyl-5H-thiazolo[3,2-a]azepinium bromide

HRID 1577771노트

반응식

HRID 1577771 반응식
C(O)(=O)C.[CH2:5]1[CH2:12][CH2:11][NH:10][C:8](=[S:9])[CH2:7][CH2:6]1.[Br:13][CH:14]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:15](O)=[O:16]>CCOCC>[Br-:13].[OH:16][C:15]1[N+:10]2[CH2:11][CH2:12][CH2:5][CH2:6][CH2:7][C:8]=2[S:9][C:14]=1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 97919Bromo(phenyl)acetic acidHCID 3003736Thiocaprolactam

생성물 1

HCID 129225446,7,8,9-Tetrahydro-3-hydroxy-2-phenyl-5H-thiazolo[3,2-a]azepinium bromide수율 86%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

An acetic acid (50 ml.) solution of ω-thiocaprolactam (6.5 g., 0.05 mole) and α-bromophenylacetic acid (10.8 g., 0.05 mole) was heated on a steam bath for 1/2 hour. The solution was first cooled and diluted with ether. Upon scratching solid which precipitated was collected. The crude material was recrystallized from acetonitrile. The purified material weighed 14 g. (86% yield) and melted at 172°-175° C.

후처리

  1. temperatureThe solution was first cooled
  2. customprecipitated
  3. customwas collected
  4. customThe crude material was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-fa8bfd2025d446bdbd73b628eeadd99d
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04289697

반응 노트

불러오는 중…