Ethanol → HCID 21258509、化合物

HRID 635350ノート

反応式

HRID 635350 の反応式
[Br:1][CH2:2][C:3]([C:5]1([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)[CH2:8][CH2:7][CH2:6]1)=O.[NH:19]1[CH2:23][CH2:22][NH:21][C:20]1=[S:24].C(O)C>C(O)(=O)C>[BrH:1].[CH:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:17]=[CH:18][C:9]=1[C:5]1([C:3]2[N:21]3[CH2:22][CH2:23][N:19]=[C:20]3[S:24][CH:2]=2)[CH2:8][CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 702EthanolHCID 2723650EthylenethioureaHCID 212584952-Bromo-1-[1-(2-naphthyl)cyclobutyl]ethanone

生成物 1

HCID 21258509HCID 21258509、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of the crude 2-bromo-1-[1-(2-naphthyl)cyclobutyl]ethanone described above, imidazolidine-2-thione (5.1 g), ethanol (60 ml) and acetic acid (40 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 a hot mixture of ethyl acetate (100 ml) and acetone (20 ml). The resulting solid was collected by filtration, washed with ethyl acetate (50 ml), dried in vacuo at 60° C., then crystallised from ethanol. The resulting solid was collected by filtration, washed with ethanol (30 ml), and dried in vacuo at 60° C. to give 3-[1-(2-naphthyl)cyclobutyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide as pale yellow prisms (10 g), m.p. 239-241° C.

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 a hot mixture of ethyl acetate (100 ml) and acetone (20 ml)
  5. filtrationThe resulting solid was collected by filtration
  6. washwashed with ethyl acetate (50 ml)
  7. customdried in vacuo at 60° C.
  8. customcrystallised from ethanol
  9. filtrationThe resulting solid was collected by filtration
  10. washwashed with ethanol (30 ml)
  11. customdried in vacuo at 60° C.

出典と根拠

ORDレコード
ord-156e456459d84c7eb20ad2eda81b4488
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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