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2-(4-Chlorophenyl)ethylamine → HCID 10039554, 화합물

HRID 374161
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반응식

HRID 374161 반응식
[C:1]([N:3]=[C:4]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)OC(C)C)#[N:2].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][NH2:24])=[CH:18][CH:17]=1>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=1)=[N:24][CH2:23][CH2:22][C:19]1[CH:20]=[CH:21][C:16]([Cl:15])=[CH:17][CH:18]=1)#[N:2]
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참가 물질

4

반응물 2

HCID 674302-(4-Chlorophenyl)ethylamineHCID 100812013-Pyridinecarboximidic acid, N-cyano-, 1-methylethyl ester

생성물 1

HCID 10039554HCID 10039554, 화합물수율 79%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Isopropyl N-cyano-3-pyridinecarboximidate (0.60 g, 3.2 mmol) was dissolved in methanol (10 ml), and 2-(4-chlorophenyl)ethylamine (0.55 g, 3.5 mmol) was added. The mixture was stirred at room temperature for 2.5 hours. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residual concentrate was subjected to chromatography on a silica gel column (WAKO GEL C-200, 50 g) eluting with chloroform-methanol (100:1). The eluted fractions were concentrated under reduced pressure, and the concentrated residue thus obtained was further crystallized from methanol-diethyl ether to give the title compound (0.71 g, 2.5 mmol, yield: 79%) as colorless powder.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. concentrationThe residual concentrate
  3. washeluting with chloroform-methanol (100:1)
  4. concentrationThe eluted fractions were concentrated under reduced pressure
  5. customthe concentrated residue thus obtained
  6. customwas further crystallized from methanol-diethyl ether

출처 및 근거

ORD 기록
ord-bafd0f783850469db5ab5757efbaec15
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05166347

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