Dichloromethane → HCID 59231917, compound

HRID 1973026Notes

Reaction equation

HRID 1973026 reaction equation
[N:1]1([CH2:7][C:8]2[N:16]3[C:11]([C:12]([NH2:17])=[N:13][CH:14]=[N:15]3)=[CH:10][CH:9]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.C(Cl)Cl.[C:28](OC([O-])=O)([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29]>C1COCC1>[NH2:17][C:12]1[C:11]2=[CH:10][CH:9]=[C:8]([CH2:7][N:1]3[CH2:6][CH2:5][N:4]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:3][CH2:2]3)[N:16]2[N:15]=[CH:14][N:13]=1

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 22064466Tert-butyldicarbonateHCID 58529836HCID 58529836, compound

Product 1

HCID 59231917HCID 59231917, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a cooled (0° C.) solution of 7-(piperazin-1-ylmethyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine (0.85 g, 3.66 mmol) and triethylamine (0.56 mL, 4.03 mmol) in THF (8.5 mL)/DCM (8.5 mL) was added iii-tert-butyl dicarbonate (0.88 g, 4.03 mmol) and the mixture was allowed to warm to rt and further stirred for 18 h and concentrated. The residue was taken up in ethyl acetate, washed with water and dried over Na2SO4 and concentrated (used in the next step without further purification). LC-MS [M+H]+=332.8, RT=1.17 min

Workup

  1. concentrationconcentrated
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated (
  5. customused in the next step without further purification)

Sources & evidence

ORD record
ord-34b8d688c52e4c99adaa74b75df2695d
Source dataset
uspto-grants-2013_04
Patent number
US08431695B2

Reaction notes

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