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

HRID 432598
ノート
印刷プレビュー

反応式

HRID 432598 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-71dbd7e58f2449e983f4a74c2a26a277
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06664258B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート