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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1-(4-chloro-2-fluoro-5-propargyloxyphenyl)-5-chloro-4-cyano-3-propyl-1,3-dihydro-2 H-imidazol-2-one → 1-(4-chloro-2-fluoro-5-propargyloxyphenyl)-4,5-dicyano-3-propyl-1,3-dihydro-2H-imidazol-2-one

HRID 465688
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인쇄 미리보기

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HRID 465688 반응식
[Cl:1][C:2]1[C:7]([O:8][CH2:9][C:10]#[CH:11])=[CH:6][C:5]([N:12]2[C:16](Cl)=[C:15]([C:18]#[N:19])[N:14]([CH2:20][CH2:21][CH3:22])[C:13]2=[O:23])=[C:4]([F:24])[CH:3]=1.[Li][C:26]#[N:27]>CN(C)C=O>[Cl:1][C:2]1[C:7]([O:8][CH2:9][C:10]#[CH:11])=[CH:6][C:5]([N:12]2[C:16]([C:26]#[N:27])=[C:15]([C:18]#[N:19])[N:14]([CH2:20][CH2:21][CH3:22])[C:13]2=[O:23])=[C:4]([F:24])[CH:3]=1
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참가 물질

4

반응물 2

HCID 198752291-(4-chloro-2-fluoro-5-propargyloxyphenyl)-5-chloro-4-cyano-3-propyl-1,3-dihydro-2 H-imidazol-2-oneHCID 178506913HCID 178506913, 화합물

생성물 1

HCID 198752701-(4-chloro-2-fluoro-5-propargyloxyphenyl)-4,5-dicyano-3-propyl-1,3-dihydro-2H-imidazol-2-one수율 45.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

The product of Example 2, 1-(4-chloro-2-fluoro5-propargyloxyphenyl)-5-chloro-4-cyano-3-propyl-1,3-dihydro-2H-imidazol-2-one (V) (0.25 g, 0.68 mmol), was stirred in 10 mL dimethylformamide (DMF). To this mixture was added LiCN (2 mL of 0.5M in DMF, 1 mmol) and the resulting mixture was heated to 120° C. for 15 minutes. The mixture was cooled poured onto water, extracted with ethyl acetate, dried, concentrated and eluted through silica gel (50:50 ethyl acetate:hexane) to give 0.11 g of 1-(4-chloro-2-fluoro-5-propargyloxyphenyl)-4,5-dicyano-3-propyl-1,3-dihydro-2H-imidazol-2-one (VI) (m.p. 76° C.).

후처리

  1. temperatureThe mixture was cooled
  2. additionpoured onto water
  3. extractionextracted with ethyl acetate
  4. customdried
  5. concentrationconcentrated
  6. washeluted through silica gel (50:50 ethyl acetate:hexane)

출처 및 근거

ORD 기록
ord-ccdbd9e339e7451eab2c4747bb55b6b4
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153316

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