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Triethylamine → 10-([1,1'-Biphenyl]-4-ylcarbonyl)-10,11-dihydrodibenz[b,f][1,4]oxazepine

HRID 1457683
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HRID 1457683 반응식
[CH:1]1[C:6]2[CH2:7][NH:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[O:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[C:23]1([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:28]=[CH:27][C:26]([C:29](Cl)=[O:30])=[CH:25][CH:24]=1>C(Cl)Cl.C(Cl)(Cl)Cl>[C:23]1([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:24]=[CH:25][C:26]([C:29]([N:8]2[CH2:7][C:6]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]2=3)=[O:30])=[CH:27][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 841514-Phenylbenzoyl chlorideHCID 64893310,11-Dihydrodibenzo(b,f)(1,4)oxazepine

생성물 1

HCID 2209956210-([1,1'-Biphenyl]-4-ylcarbonyl)-10,11-dihydrodibenz[b,f][1,4]oxazepine수율 83.6%

시약·촉매·용매 2

HCID 6212Chloroform용매
HCID 6344
Dichloromethane
용매

실험 절차

To a cooled (0° C.) solution of 1.0 g of 10,11-dihydrodibenz[b,f][1,4]oxazepine and 7 ml of triethylamine in 30 ml of CH2Cl2 under argon is added dropwise 2.0 g of [1,1'-biphenyl]-4-carbonyl chloride. The mixture is stirred at room temperature for 16 hours and diluted with 50 ml of CHCl3. The mixture is washed with 30 ml each of H2O, 2NHCl, H2O, saturated NaHCO3, H2O, and dried (Na2SO4). Solvent is removed under vacuum to give 1.6 g of a yellow solid, m.p. 93°-95° C; Mass spectrum (CI), 378(MH+).

후처리

  1. washThe mixture is washed with 30 ml each of H2O
  2. dry with material2NHCl, H2O, saturated NaHCO3, H2O, and dried (Na2SO4)
  3. customSolvent is removed under vacuum

출처 및 근거

ORD 기록
ord-31023d15da084e1383be49dffd1f81a4
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849735

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