Carbon Disulfide → (RS)-9,9a-dihydrothiazolo[3,4-a]indole-3-thione

HRID 262121노트

반응식

HRID 262121 반응식
[C:1](=[S:3])=[S:2].OS(O[CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[NH:11]1)(=O)=O>[OH-].[Na+]>[CH2:9]1[CH:10]2[CH2:18][C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]2[C:1](=[S:3])[S:2]1

참가 물질

4

반응물 2

HCID 6348Carbon DisulfideHCID 21320152(RS)-2-hydroxysulphonyloxymethylindoline

생성물 1

HCID 21320146(RS)-9,9a-dihydrothiazolo[3,4-a]indole-3-thione

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
20 °C

실험 절차

Carbon disulphide (65 cc) is added to a suspension of (RS)-2-hydroxysulphonyloxymethylindoline (45.8 g) in 1.5 N aqueous sodium hydroxide solution (400 cc). After stirring for 2 hours at a temperature of about 20° C., a solution is obtained and the formation of beige crystals is then observed; stirring is continued for 12 hours. The crystals formed are filtered off, washed with water and then recrystallised from ethanol (850 cc). (RS)-9,9a-dihydrothiazolo[3,4-a]indole-3-thione (31.3 g) is thus obtained in the form of white crystals melting at 132° C.

후처리

  1. customa solution is obtained
  2. stirringstirring
  3. waitis continued for 12 hours
  4. customThe crystals formed
  5. filtrationare filtered off
  6. washwashed with water
  7. customrecrystallised from ethanol (850 cc)

출처 및 근거

ORD 기록
ord-1fd7ba3f4027423f97d94b5e29a5d35e
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04153699

반응 노트

불러오는 중…