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3-Fluoroaniline → HCID 178509198、化合物

HRID 2304446
ノート
印刷プレビュー

反応式

HRID 2304446 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:8][N:9]=[C:10]([C:13]#[N:14])[C:11]#[N:12])[CH:5]=[CH:6][CH:7]=1.FC1C=C(C=CC=1)N.C(CC(OC1CCCCC1)=O)#N.[OH2:35].[NH2:36]N>C(O)C>[NH2:14][C:13]1[C:10](=[N:9][NH:8][C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=2)[C:11](=[O:35])[NH:12][N:36]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 97423-FluoroanilineHCID 24654Hydrazine hydrate (1:1)HCID 96357Cyclohexyl cyanoacetateHCID 4199695HCID 4199695、化合物

生成物 1

HCID 178509198HCID 178509198、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

This compound was prepared using 2-[(3-fluorophenyl)hydrazono]malononitrile (145 mg, 0.5 mmole), which was derived from 3-fluoroaniline (111 mg, 1 mmole)) and cyclohexyl cyanoacetate (217 mg, 1.3 mmole) as described in Example 8, and hydrazine hydrate (25 mg, 0.5 mmole) in ethanol. Solids had not formed after heating the reaction at 80° C. for 40 minutes, however, analysis of the reaction solution by TLC indicated that no starting material remained. The solution was allowed to cool to room temperature and concentrated. The product was obtained after filtration as a yellow solid (73 mg). 1H NMR (ppm, DMSO-d6): 5.95 (br., s, 2H), 6.90 (m, 1H), 7.20-7.65 (m, 3H), 10.56 (br., s, 1H) 12.77 (br., s, 1H).

後処理

  1. customThis compound was prepared
  2. customSolids had not formed
  3. temperatureafter heating
  4. customthe reaction at 80° C. for 40 minutes
  5. concentrationconcentrated
  6. customThe product was obtained
  7. filtrationafter filtration as a yellow solid (73 mg)

出典と根拠

ORDレコード
ord-c2ceccb492f845e68b224ee6ec0a4124
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06436915B1

反応ノート

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