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Phenyl isocyanate → N-[4-(2-diethylaminoethoxy)phenyl]-N-[4,5-dihydro-1-phenyl-1H-pyrazol-3-yl]-N'-phenylurea

HRID 1031951
ノート
印刷プレビュー

反応式

HRID 1031951 の反応式
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:10]([N:12]([CH2:34][CH3:35])[CH2:13][CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]2[CH2:27][CH2:26][N:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[N:24]=2)=[CH:18][CH:17]=1)[CH3:11]>O1CCCC1>[CH2:34]([N:12]([CH2:10][CH3:11])[CH2:13][CH2:14][O:15][C:16]1[CH:17]=[CH:18][C:19]([N:22]([C:23]2[CH2:27][CH2:26][N:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[N:24]=2)[C:8]([NH:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:9])=[CH:20][CH:21]=1)[CH3:35]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7672Phenyl isocyanateHCID 178464081HCID 178464081、化合物

生成物 1

HCID 22167070N-[4-(2-diethylaminoethoxy)phenyl]-N-[4,5-dihydro-1-phenyl-1H-pyrazol-3-yl]-N'-phenylurea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Phenylisocyanate (1.05 ml) was added dropwise to a solution of N-[4-(2-diethylaminoethoxy)phenyl]-4,5-dihydro-1-phenyl-1H-pyrazol-3-amine (2.4 g) in tetrahydrofuran (30 ml) and the solution heated to reflux for 4 hours. After cooling the solvent was removed and water added to the residue, which was then extracted with ether. The combined ether layer was washed with water and dried. Solvent was removed to give a solid which was recrystallised from ethyl acetate and petroleum ether to give the title compound (1.3 g) mp 140°-1°.

後処理

  1. temperaturethe solution heated
  2. temperatureto reflux for 4 hours
  3. temperatureAfter cooling the solvent
  4. customwas removed
  5. additionwater added to the residue, which
  6. extractionwas then extracted with ether
  7. washThe combined ether layer was washed with water
  8. customdried
  9. customSolvent was removed
  10. customto give a solid which
  11. customwas recrystallised from ethyl acetate and petroleum ether

出典と根拠

ORDレコード
ord-e182dbdf1ef8449dad3f0f622cf63da2
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04956378

反応ノート

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