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Ethanol → 2-(4-Chlorophenyl)-3-[1-(3,4-dichlorophenyl)cyclobutyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide

HRID 635364
ノート
印刷プレビュー

反応式

HRID 635364 の反応式
[Br:1][CH:2]([C:17]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=1)[C:3]([C:5]1([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[C:11]([Cl:16])[CH:10]=2)[CH2:8][CH2:7][CH2:6]1)=O.[NH:24]1[CH2:28][CH2:27][NH:26][C:25]1=[S:29].C(O)C>C(O)(=O)C>[BrH:1].[Cl:23][C:20]1[CH:21]=[CH:22][C:17]([C:2]2[S:29][C:25]3=[N:24][CH2:28][CH2:27][N:26]3[C:3]=2[C:5]2([C:9]3[CH:14]=[CH:13][C:12]([Cl:15])=[C:11]([Cl:16])[CH:10]=3)[CH2:8][CH2:7][CH2:6]2)=[CH:18][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 2723650EthylenethioureaHCID 212583922-Bromo-2-(4-chlorophenyl)1-[1-(3,4-dichlorophenyl)cyclobutyl]ethanone

生成物 1

HCID 212584932-(4-Chlorophenyl)-3-[1-(3,4-dichlorophenyl)cyclobutyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide収率 21.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 2-bromo-2-(4-chlorophenyl)1-[1-(3,4-dichlorophenyl)cyclobutyl]ethanone (3.68 g), imidazolidine-2-thione (0.87 g), ethanol (60 ml) and acetic acid (35 ml) was heated under reflux for 18 hours then allowed to cool to ambient temperature. The solvents were removed in vacuo and the residue was triturated with ethanol (30 ml). The resulting solid was collected by filtration and crystallised from acetic acid. The resulting product was collected by filtration, washed with acetic acid (10 ml) and dried in vacuo at 100° C. to give 2-(4-chlorophenyl)-3-[1-(3,4-dichlorophenyl)cyclobutyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide as a colourless solid (0.93 g), m.p. 302-304° C. (decomposes).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customThe solvents were removed in vacuo
  4. customthe residue was triturated with ethanol (30 ml)
  5. filtrationThe resulting solid was collected by filtration
  6. customcrystallised from acetic acid
  7. filtrationThe resulting product was collected by filtration
  8. washwashed with acetic acid (10 ml)
  9. customdried in vacuo at 100° C.

出典と根拠

ORDレコード
ord-15557f8a0bac45938342ef6fdde98d1f
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06187802B1

反応ノート

読み込み中…

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