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Hydrochloric Acid → HCID 57829289、化合物

HRID 2356697
ノート
印刷プレビュー

反応式

HRID 2356697 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 57829289HCID 57829289、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0a21e7d0d3a141f18ea0d6e16d947040
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759366B2

反応ノート

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