Hydrochloric Acid → 4-(1-Benzyl-piperidin-4-ylidenemethyl)-benzimidic acid ethyl ester

HRID 1663237ノート

反応式

HRID 1663237 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]2[CH:22]=[CH:21][C:18]([C:19]#[N:20])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(Cl)(Cl)Cl.Cl.[CH2:28]([OH:30])[CH3:29]>>[CH2:28]([O:30][C:19](=[NH:20])[C:18]1[CH:17]=[CH:16][C:15]([CH:14]=[C:11]2[CH2:12][CH2:13][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9][CH2:10]2)=[CH:22][CH:21]=1)[CH3:29]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 6212ChloroformHCID 674356554-(1-Benzyl-piperidin-4-ylidenemethyl)-benzonitrile

生成物 1

HCID 674362034-(1-Benzyl-piperidin-4-ylidenemethyl)-benzimidic acid ethyl ester収率 92.4%

実験手順

A mixture of 4-(1-benzyl-piperidin-4-ylidenemethyl)-benzonitrile (14 g, 48.6 mmol), chloroform (10 mL) and 6 M hydrogen chloride in ethanol (300 mL) was stirred at room temperature for 48 hours. The solution was concentrated in vacuo, the remaining solid was repeatedly dissolved in ethanol (400 mL) and concentrated in vacuo to yield 16.4 g (92.4%) of the title compound, which was used in the next steps without further purification.

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. dissolutionthe remaining solid was repeatedly dissolved in ethanol (400 mL)
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-491d251fbdd64308bae3659291581e66
出典データセット
uspto-grants-2011_10
特許番号
US08034827B2

反応ノート

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