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Sodium hydride → 1H-Indole-7-propanenitrile, 1-[[3-[2-(7-chloro-2-quinolinyl)ethenyl]phenyl]methyl]-, (E)-

HRID 1198541
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HRID 1198541 반응식
[C:1]([CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:13]=1[NH:12][CH:11]=[CH:10]2)#[N:2].[H-].[Na+].[Cl:16][C:17]1[CH:26]=[C:25]2[C:20]([CH:21]=[CH:22][C:23](/[CH:27]=[CH:28]/[C:29]3[CH:30]=[C:31]([CH:34]=[CH:35][CH:36]=3)[CH2:32]Cl)=[N:24]2)=[CH:19][CH:18]=1.[Cl-].[NH4+]>CN(C)C=O>[C:1]([CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:13]=1[N:12]([CH2:32][C:31]1[CH:34]=[CH:35][CH:36]=[C:29](/[CH:28]=[CH:27]/[C:23]3[CH:22]=[CH:21][C:20]4[C:25](=[CH:26][C:17]([Cl:16])=[CH:18][CH:19]=4)[N:24]=3)[CH:30]=1)[CH:11]=[CH:10]2)#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 19369489trans-3-[2-(7-Chloroquinolin-2-yl)ethenyl]benzyl chlorideHCID 199591053-(1H-Indol-7-YL)propanenitrile

생성물 1

HCID 191026011H-Indole-7-propanenitrile, 1-[[3-[2-(7-chloro-2-quinolinyl)ethenyl]phenyl]methyl]-, (E)-

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
3회

실험 절차

A solution of 7-(2-cyanoethyl)indole (Example 14a) (4.42 g, 26 mmol) in dimethylformamide (30 ml) was added dropwise to a stirred suspension of sodium hydride (1.3 g, 60% dispersion, 32.5 mmol, washed with hexane under nitrogen) in dimethylformamide (30 ml) at 10°-15° C. The mixture was stirred for 15 minutes at ca 15° C. then a suspension of 3-[2(E)-(7-chloroquinolin-2-yl)ethenyl] benzyl chloride (Example 14b) (10.2 g, 32.5 mmol) in dimethylformamide (60 ml) was added rapidly. The dark mixture was stirred for 5 hours at room temperature, poured onto saturated ammonium chloride solution and extracted with dichloromethane. The extract was dried and evaporated under high vacuum and the residue in dichloromethane (30 ml) was applied to a silica column and eluted with ethyl acetate-hexane (1:2). The product was recrystallised from ethyl acetate-hexane, m.p. 151° C.

후처리

  1. additionwas added rapidly
  2. stirringThe dark mixture was stirred for 5 hours at room temperature
  3. extractionextracted with dichloromethane
  4. customThe extract was dried
  5. customevaporated under high vacuum
  6. washeluted with ethyl acetate-hexane (1:2)
  7. customThe product was recrystallised from ethyl acetate-hexane, m.p. 151° C.

출처 및 근거

ORD 기록
ord-f6249be6704b456aaa971ddb5179a7e7
출처 데이터셋
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05281593

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