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

HRID 1663237노트

반응식

HRID 1663237 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-491d251fbdd64308bae3659291581e66
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034827B2

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