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Hydrochloric Acid → 2-Fluoro-4-(piperazin-1-YL)benzonitrile

HRID 432598
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HRID 432598 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]#[N:21])=[C:16]([F:22])[CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CO>[F:22][C:16]1[CH:15]=[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:19]=[CH:18][C:17]=1[C:20]#[N:21]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 54552536Tert-butyl 4-(4-cyano-3-fluorophenyl)piperazine-1-carboxylate

생성물 1

HCID 187600452-Fluoro-4-(piperazin-1-YL)benzonitrile

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4-(4-cyano-3-fluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (6.97 g, 22.83 mmol) in methanol (250 mL) was saturated with HCl gas and stirred at ambient temperature overnight. The reaction was concentrated, saturated sodium bicarbonate (250 mL) was added and the slurry was stirred for 1 hour. The resulting solid was filtered off, rinsed well with water, air dried then evacuated overnight. As water was removed from the solid, it turned to a milky yellow solid which slowly solidified to give 2-fluoro-4-piperazin-1-yl-benzonitrile as a waxy solid (3.84 g, 82%).

후처리

  1. concentrationThe reaction was concentrated
  2. additionsaturated sodium bicarbonate (250 mL) was added
  3. stirringthe slurry was stirred for 1 hour
  4. filtrationThe resulting solid was filtered off
  5. washrinsed well with water, air
  6. customdried
  7. customthen evacuated overnight
  8. customAs water was removed from the solid, it

출처 및 근거

ORD 기록
ord-71dbd7e58f2449e983f4a74c2a26a277
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06664258B1

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