Ethanol → 3-(4-Chlorobenzo[b]thiophen-2-yl)-2-ethyl-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide

HRID 2183645ノート

反応式

HRID 2183645 の反応式
[Br:1][CH:2]([CH2:15][CH3:16])[C:3]([C:5]1[S:9][C:8]2[CH:10]=[CH:11][CH:12]=[C:13]([Cl:14])[C:7]=2[CH:6]=1)=O.[NH:17]1[CH2:21][CH2:20][NH:19][C:18]1=[S:22].C(O)C>C(O)(=O)C>[BrH:1].[Cl:14][C:13]1[C:7]2[CH:6]=[C:5]([C:3]3[N:19]4[CH2:20][CH2:21][N:17]=[C:18]4[S:22][C:2]=3[CH2:15][CH3:16])[S:9][C:8]=2[CH:10]=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 702EthanolHCID 2723650EthylenethioureaHCID 224739972-Bromo-1-(4-chlorobenzo[b]thiophen-2-yl)butan-1-one

生成物 1

HCID 224738223-(4-Chlorobenzo[b]thiophen-2-yl)-2-ethyl-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide収率 71.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 2-bromo-1-(4-chlorobenzo[b]thiophen-2-yl)butan-1-one (1.06 g), 2-imidazolidinethione (0.255 g) and ethanol (25 ml) was heated under reflux for 20 minutes. Acetic acid (12 ml) was added, the mixture was heated under reflux for 21 hours, then the solvents were removed in vacuo and the solid residue recrystallised from propan-2-ol (40 ml) to give 3-(4-chlorobenzo[b]thiophen-2-yl)-2-ethyl-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide (0.72 g) as a white solid, m.p. 187-189° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 minutes
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for 21 hours
  5. customthe solvents were removed in vacuo
  6. customthe solid residue recrystallised from propan-2-ol (40 ml)

出典と根拠

ORDレコード
ord-67c19d293d4f43d8bafa21e1ac13f0dd
出典データセット
uspto-grants-2005_05
特許番号
US06900216B2

反応ノート

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