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

HRID 262121ノート

反応式

HRID 262121 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-1fd7ba3f4027423f97d94b5e29a5d35e
出典データセット
uspto-grants-1979_05
特許番号
US04153699

反応ノート

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