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Ammonium Chloride → HCID 178428440, 화합물

HRID 1445108
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HRID 1445108 반응식
[N-:1]=[N+:2]=[N-:3].[Na+].[Cl:5][C:6]1[CH:7]=[C:8]([CH:33]=[CH:34][CH:35]=1)[CH2:9][N:10]1[C:14]2=[C:15]([N:21]3[CH2:30][CH2:29][C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[CH2:22]3)[N:16]=[C:17]([C:19]#[N:20])[CH:18]=[C:13]2[C:12]([CH3:31])=[C:11]1[CH3:32].[Cl-].[NH4+].N([O-])=O.[Na+]>CN(C)C=O>[Cl:5][C:6]1[CH:7]=[C:8]([CH:33]=[CH:34][CH:35]=1)[CH2:9][N:10]1[C:14]2=[C:15]([N:21]3[CH2:30][CH2:29][C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[CH2:22]3)[N:16]=[C:17]([C:19]3[NH:20][N:3]=[N:2][N:1]=3)[CH:18]=[C:13]2[C:12]([CH3:31])=[C:11]1[CH3:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 23668193Sodium NitriteHCID 67141952HCID 67141952, 화합물

생성물 1

HCID 178428440HCID 178428440, 화합물수율 33.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium azide (137 mg, 2.1 mmol) was added at 0° C. to a solution of 1-(3-chlorobenzyl)-7-(3,4-dihydro-1H-isoquinolin-2-yl)-2,3-dimethyl-1H-pyrrolo[2,3-c]pyridin-5-carbonitrile (300 mg, 0.7 mmol) prepared in Example 689 and ammonium chloride (74.9 mg, 1.4 mmol) in anhydrous N,N-dimethylformamide (10 ml). The reaction mixture was refluxed overnight. 6% sodium nitrite solution was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was dried on anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified with silica gel column chromatography (ethyl acetate/n-hexane=1/3, v/v) to give 110 mg of the titled compound as a white solid. (Yield: 33%).

후처리

  1. temperatureThe reaction mixture was refluxed overnight
  2. extractionwas then extracted with ethyl acetate
  3. dry with materialThe organic layer was dried on anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified with silica gel column chromatography (ethyl acetate/n-hexane=1/3

출처 및 근거

ORD 기록
ord-4bab9a874c6244608e273c98ce175992
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662832B2

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