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

3-Methoxypropylamine → Tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate

HRID 1921980
Notes
Print preview

Reaction equation

HRID 1921980 reaction equation
Br[CH2:2][CH2:3][CH2:4][NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[C:8]([C:18]2[CH:23]=[CH:22][N:21]=[C:20]([NH:24][CH3:25])[N:19]=2)[CH:7]=1.[CH3:26][O:27][CH2:28][CH2:29][CH2:30][NH2:31].[C:32](=O)([O:38]C(C)(C)C)[O:33][C:34]([CH3:37])([CH3:36])[CH3:35].C(N(CC)CC)C>CN(C)C(=O)C>[CH3:17][O:16][C:13]1[CH:14]=[C:15]2[C:10]([CH:9]=[C:8]([C:18]3[CH:23]=[CH:22][N:21]=[C:20]([NH:24][CH3:25])[N:19]=3)[CH:7]=[C:6]2[NH:5][CH2:4][CH2:3][CH2:2][N:31]([CH2:30][CH2:29][CH2:28][O:27][CH3:26])[C:32](=[O:38])[O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[CH:11][CH:12]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 16723-MethoxypropylamineHCID 8471TriethylamineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 532581654-(4-((3-bromopropyl)amino)-6-methoxynaphthalen-2-yl)-N-methylpyrimidin-2-amine

Product 1

HCID 67307853Tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate
Yield 39.2%

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Procedure

A mixture of 4-(4-((3-bromopropyl)amino)-6-methoxynaphthalen-2-yl)-N-methylpyrimidin-2-amine (189) (0.10 g, 0.25 mmol) and N,N-dimethylacetamide (2 mL) were treated with 3-methoxypropan-1-amine (0.10 mL, 1.0 mmol). The resulting mixture was stirred at room temperature 16 h. The reaction mixture was dried down and treated with di-tert-butyl carbonate solution (1 mL of 0.6 M solution in methanol, 0.6 mmol) and triethylamine (0.5 mL, 3.6 mmol). The resulting mixture was stirred at room temperature for 16 h. The reaction mixture was concentrated (rotary) and dissolved in ethyl acetate (20 mL) and water (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organics were dried over Na2SO4, filtered and concentrated (rotary). The residue was purified by column chromatography (silica gel) using 85% ethyl acetate/hexanes as the eluent to afford tert-butyl (3-((7-methoxy-3-(2-(methylamino)pyrimidin-4-yl)naphthalen-1-yl)amino)propyl)(3-methoxypropyl)carbamate (190) as an orange oil (0.05 g). The residue was dissolved in dioxane (1 mL) and then treated with HCl (4 M in dioxane, 0.5 mL, 7.2 mmol). The reaction mixture was stirred at room temperature and then filtered to afford N-{7-methoxy-3-[2-(methylamino)pyrimidin-4-yl]-1-naphthyl}-N′-(3-methoxypropyl)propane-1,3-diamine was isolated as a red-orange solid. M.p.=130-132° C. 400 MHz 1H NMR (DMSO-d6) δ: 8.88 (br s, 2H), 8.44 (d, J=6.3 Hz, 1H), 8.11 (br s, 1H), 7.90 (d, J=9.0 Hz, 1H), 7.66-7.56 (m, 2H), 7.28-7.24 (m, 2H), 3.96 (s, 3H), 3.56-3.41 (m, 4H), 3.22 (s, 3H), 3.20-2.95 (m, 7H); Experimental Elemental Analysis (3.2 equivalents of HCl)=52.49% C, 6.19% H, 12.82% N; Calculated Elemental Analysis 52.50% C, 6.55% H, 13.31% N; LCMS (m/z): 410 [M+H].

Workup

  1. customThe reaction mixture was dried down
  2. stirringThe resulting mixture was stirred at room temperature for 16 h
  3. concentrationThe reaction mixture was concentrated (rotary)
  4. dissolutiondissolved in ethyl acetate (20 mL)
  5. extractionThe aqueous layer was extracted with ethyl acetate (2×10 mL)
  6. dry with materialThe combined organics were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated (rotary)
  9. customThe residue was purified by column chromatography (silica gel)

Sources & evidence

ORD record
ord-ac88514fcc75401e8891789eed6b13fb
Source dataset
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08173808B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes