HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Triethylamine → N-cyano-N'-(4-methylthiobenzyl)-4-pyridinecarboximidamide

HRID 1588550
Notes
Print preview

Reaction equation

HRID 1588550 reaction equation
[C:1]([N:3]=[C:4]([C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)OC(C)C)#[N:2].Cl.[CH3:16][S:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22][NH2:23])=[CH:20][CH:19]=1.C(N(CC)CC)C>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[CH:11][N:12]=[CH:13][CH:14]=1)=[N:23][CH2:22][C:21]1[CH:24]=[CH:25][C:18]([S:17][CH3:16])=[CH:19][CH:20]=1)#[N:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 10012715Isopropyl N-cyano-4-pyridinecarboximidateHCID 19734486[4-(Methylsulfanyl)phenyl]methanamine hydrochloride

Product 1

HCID 19734494N-cyano-N'-(4-methylthiobenzyl)-4-pyridinecarboximidamideYield 49%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Isopropyl N-cyano-4-pyridinecarboximidate (0.40 g, 2.1 mmol) was dissolved in methanol (15 ml), and 4-methylthiobenzylamine hydrochloride (0.60 g, 3.2 mmol) and triethylamine (0.43 g, 4.2 mmol) were added. The mixture was stirred at room temperature for 1 hour. After the reaction was completed, the reaction solution was then concentrated under reduced pressure. The residual concentrate was extracted with ethyl acetate (50 ml×3). The ethyl acetate layer was washed with water (100 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residual concentrate was crystallized from methanol-diethyl ether to give the title compound (0.29 g, 1.0 mmol, yield: 49%) as colorless crystals.

Workup

  1. concentrationthe reaction solution was then concentrated under reduced pressure
  2. concentrationThe residual concentrate
  3. extractionwas extracted with ethyl acetate (50 ml×3)
  4. washThe ethyl acetate layer was washed with water (100 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. concentrationThe residual concentrate
  8. customwas crystallized from methanol-diethyl ether

Sources & evidence

ORD record
ord-bcc41c357f66448fa8c06a86a542395e
Source dataset
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05223508

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes