Triethylamine → HCID 10366274, 화합물

HRID 36921노트

반응식

HRID 36921 반응식
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]

참가 물질

6

반응물 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

생성물 1

HCID 10366274HCID 10366274, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f4146c2cd77f4afda0fd0c09ba362881
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418239

반응 노트

불러오는 중…