Triethylamine → HCID 10366274、化合物

HRID 258029ノート

反応式

HRID 258029 の反応式
C([N:3]([CH2:6]C)CC)C.[CH3:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[C:20]2[CH:21]=[C:22]3[CH2:27][CH2:26][CH2:25][C:23]3=[CH:24][C:19]=2[O:18][C:17](=[O:28])[C:16]=1C(O)=O.C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:39])=CC=1.[F:49][C:50]1[CH:56]=[C:55]([F:57])[CH:54]=[CH:53][C:51]=1[NH2:52]>C1C=CC=CC=1>[F:49][C:50]1[CH:56]=[C:55]([F:57])[CH:54]=[CH:53][C:51]=1[NH:52][C:6]([NH:3][C:16]1[C:17](=[O:28])[O:18][C:19]2[CH:24]=[C:23]3[CH2:25][CH2:26][CH2:27][C:22]3=[CH:21][C:20]=2[C:15]=1[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[CH3:8])=[O:39]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 97092,4-DifluoroanilineHCID 199401P,P-Diphenylphosphinic azideHCID 103586304-(2-Methylphenyl)-2-oxo-2,6,7,8-tetrahydrocyclopenta[g][1]benzopyran-3-carboxylic acid

生成物 1

HCID 10366274HCID 10366274、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Triethylamine (1.2 ml) was added dropwise to a mixture of 4-(2-methylphenyl)-2-oxo-2,6,7,8-tetrahydrocyclopenta[g][1]benzopyran-3-carboxylic acid (2.56 g), DPPA (2.64 g) and benzene (32 ml). The mixture was stirred at room temperature for 30 minutes and, then, on reflux for 30 minutes. Then, 2,4-difluoroaniline (1.0 ml) was added and the mixture was further refluxed for 30 minutes. The reaction mixture was washed with water, 1N HCl and water in the order mentioned and, then, dried (MgSO4). The solvent was then distilled off to give N-(2,4-difluorophenyl)-N'-[4-(2-methylphenyl)-2-oxo-2,6,7,8-tetrahydrocyclopenta[g][1]-benzopyran-3-yl]urea as oil. The oil was crystallized by addition of isopropyl ether (3.4 g, 95.2%). Recrystallization from acetone gave colorless prisms, m.p. 223°-224° C.

後処理

  1. temperatureon reflux for 30 minutes
  2. temperaturethe mixture was further refluxed for 30 minutes
  3. washThe reaction mixture was washed with water, 1N HCl and water in the order
  4. dry with materialdried (MgSO4)
  5. distillationThe solvent was then distilled off

出典と根拠

ORDレコード
ord-51453e7c03734faf9b2473b1a5131b1d
出典データセット
uspto-grants-1993_11
特許番号
US05264454

反応ノート

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