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Hydrochloric Acid → HCID 57829289, 화합물

HRID 2356697
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HRID 2356697 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:18])[NH:10][C:11]([CH3:17])([CH3:16])[C:12](OC)=[O:13])=[CH:4][C:3]=1[C:19]1[S:20][CH:21]=[CH:22][CH:23]=1.Cl>O1CCCC1.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH3:17])([CH3:16])[NH:10][C:9]2=[O:18])=[CH:4][C:3]=1[C:19]1[S:20][CH:21]=[CH:22][CH:23]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 57829328Methyl 2-[3-(4-fluoro-3-thiophen-2-ylphenyl)ureido]-2-methylpropionate

생성물 1

HCID 57829289HCID 57829289, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

0.62 g of compound 267.3 was dissolved at room temperature in 5 ml of dry tetrahydrofuran, admixed with 0.62 ml of concentrated hydrochloric acid and stirred at 80° C. for 2 h. The cooled reaction mixture was taken up in ethyl acetate and washed with saturated sodium hydrogencarbonate solution, and the organic phase was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was stirred with diisopropyl ether, filtered and dried. 3-(4-Fluoro-3-thiophen-2-yl-phenyl)-5,5-dimethylimidazolidine-2,4-dione (267.2) was obtained. Molecular weight 304.06 (C15H13FN2O2S); retention time Rt=2.25 min. [E]; MS (ESI): 346.09 (MH++CH3CN).

후처리

  1. customThe cooled reaction mixture
  2. washwashed with saturated sodium hydrogencarbonate solution
  3. dry with materialthe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. stirringThe residue was stirred with diisopropyl ether
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-0a21e7d0d3a141f18ea0d6e16d947040
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759366B2

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