Ethanol → 3-(Benzo[b]furan-3-yl)-5,6-dihydroimidazo[2,1-b]thiazole monohydrobromide

HRID 362260

반응식

HRID 362260 반응식
[Br:1][CH2:2][C:3]([C:5]1[C:6]2[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=2[O:8][CH:9]=1)=O.[NH:14]1[CH2:18][CH2:17][NH:16][C:15]1=[S:19].C(O)C>C(O)(=O)C>[BrH:1].[O:8]1[CH:9]=[C:5]([C:3]2[N:16]3[CH2:17][CH2:18][N:14]=[C:15]3[S:19][CH:2]=2)[C:6]2[CH:13]=[CH:12][CH:11]=[CH:10][C:7]1=2

참가 물질

5

반응물 3

HCID 702EthanolHCID 2723650EthylenethioureaHCID 27765801-(Benzofuran-3-yl)-2-bromoethanone

생성물 1

HCID 702844723-(Benzo[b]furan-3-yl)-5,6-dihydroimidazo[2,1-b]thiazole monohydrobromide수율 56.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 3-(2-bromoacetyl)benzo[b]furan (36.9 g), 2-imidazolidinethione (15.75 g), ethanol (600 ml) and acetic acid (400 ml) was heated under reflux for 21 hours then allowed to cool to ambient temperature. The resulting solid was collected by filtration, washed with ether (500 ml), and dissolved in hot methanol (500 ml). Charcoal (2 g) was added and the hot mixture was stirred for a few minutes, then filtered and allowed to cool to ambient temperature. The resulting solid was collected by filtration, ground to a fine powder, and dried in vacuo at 80° C. to give 3-(benzo[b]furan-3-yl)-5,6-dihydroimidazo[2,1-b]thiazole monohydrobromide 0.7 hydrate as an off-white solid (28.1 g), m.p. 251°-254.50C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 21 hours
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with ether (500 ml)
  5. dissolutiondissolved in hot methanol (500 ml)
  6. additionCharcoal (2 g) was added
  7. filtrationfiltered
  8. temperatureto cool to ambient temperature
  9. filtrationThe resulting solid was collected by filtration, ground to a fine powder
  10. customdried in vacuo at 80° C.

출처 및 근거

ORD 기록
ord-23c8818a734b430cb18040dd1fe1757f
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05869492

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