Ethanol → 3-[1-(3,4-Dichlorophenyl)cyclopentyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide

HRID 635352ノート

反応式

HRID 635352 の反応式
[Br:1][CH2:2][C:3]([C:5]1([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=2)[CH2:9][CH2:8][CH2:7][CH2:6]1)=O.[NH:18]1[CH2:22][CH2:21][NH:20][C:19]1=[S:23].C(O)C>C(O)(=O)C>[BrH:1].[Cl:17][C:12]1[CH:11]=[C:10]([C:5]2([C:3]3[N:20]4[CH2:21][CH2:22][N:18]=[C:19]4[S:23][CH:2]=3)[CH2:9][CH2:8][CH2:7][CH2:6]2)[CH:15]=[CH:14][C:13]=1[Cl:16]

参加物

5

反応物 3

HCID 702EthanolHCID 2723650EthylenethioureaHCID 212585122-Bromo-1-[1-(3,4-dichlorophenyl)cyclopentyl]ethanone

生成物 1

HCID 212584093-[1-(3,4-Dichlorophenyl)cyclopentyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 2-bromo-1-[1-(3,4-dichlorophenyl)cyclopentyl]ethanone (0.5 g), imidazolidine-2-thione (0.16 g), ethanol (3 ml) and acetic acid (2 ml) was heated under reflux for 18 hours then allowed to cool to ambient temperature. The solvents were removed in vacuo and the residue crystallised from a 1:1 mixture of ethyl acetate and ethanol. The resulting product was collected by filtration, washed with ethanol (3 ml) and dried in vacuo at 60° C. to give 3-[1-(3,4-dichlorophenyl)cyclopentyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide as white microneedles (0.27 g), m.p. 230-232° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customThe solvents were removed in vacuo
  4. customthe residue crystallised from a 1:1 mixture of ethyl acetate and ethanol
  5. filtrationThe resulting product was collected by filtration
  6. washwashed with ethanol (3 ml)
  7. customdried in vacuo at 60° C.

出典と根拠

ORDレコード
ord-c910e2123d8c44a8b4fa76c3ac018f61
出典データセット
uspto-grants-2001_02
特許番号
US06187802B1

反応ノート

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