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Sodium Hydroxide → 4-[4-[(1H-Benzotriazol-1-Yl)Oxy]-8-Chloro-5,6-Dihydro-11H-Benzo[5,6]Cyclohepta[1,2-b]Pyridin-11-Ylidene]-1-(3-Pyridinylacetyl)-Piperidine

HRID 1940670
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HRID 1940670 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[C:8](=[C:18]3[CH2:23][CH2:22][N:21]([C:24](=[O:32])[CH2:25][C:26]4[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=4)[CH2:20][CH2:19]3)[C:9]3[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:10]=3[CH2:11][CH2:12][C:3]=12.[CH:33]1[CH:34]=[CH:35][C:36]2[N:41]([OH:42])[N:40]=[N:39][C:37]=2[CH:38]=1.[H-].[Na+].[OH-].[Na+]>CN(C)C=O.O>[N:41]1([O:42][C:2]2[CH:7]=[CH:6][N:5]=[C:4]3[C:8](=[C:18]4[CH2:23][CH2:22][N:21]([C:24](=[O:32])[CH2:25][C:26]5[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=5)[CH2:20][CH2:19]4)[C:9]4[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:10]=4[CH2:11][CH2:12][C:3]=23)[C:36]2[CH:35]=[CH:34][CH:33]=[CH:38][C:37]=2[N:39]=[N:40]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 757711-HydroxybenzotriazoleHCID 226219554-[4,8-Dichloro-5,6-Dihydro-11H-Benzo[5,6]Cyclohepta[1,2-b]Pyridin-11-Ylidene]-1-(3-Pyridinylacetyl)-Piperidine

생성물 1

HCID 226219504-[4-[(1H-Benzotriazol-1-Yl)Oxy]-8-Chloro-5,6-Dihydro-11H-Benzo[5,6]Cyclohepta[1,2-b]Pyridin-11-Ylidene]-1-(3-Pyridinylacetyl)-Piperidine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
25 °C

실험 절차

The 4,8-dichloro compound from Example 250 (0.8 grams) was added to a solution of HOBT (1.2 grams) and sodium hydride (0.14 grams, 60% in mineral oil) in anhydrous dimethyl-formamide (60 mL). The resulting solution was irradiated with a 200 W lamp while stirring at 25° C. for 60 hours. The solution was poured into 1N aqueous NaOH while stirring and an additional 400 mL of water was added to the resulting mixture. Filtration provided a solid which was washed with water several times. The solid was dissolved in CH2Cl2 -acetone, dried over anhydrous MgSO4, and concentrated in vacuo to proved the title compound (0.87 grams, 90%, mp=120°-122° C., MH+ 563).

후처리

  1. customThe resulting solution was irradiated with a 200 W lamp
  2. stirringwhile stirring
  3. filtrationFiltration
  4. customprovided a solid which
  5. washwas washed with water several times
  6. dissolutionThe solid was dissolved in CH2Cl2 -acetone
  7. dry with materialdried over anhydrous MgSO4
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2e5bac1cbcc9401fbb76e08d8aca6d3a
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700806

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