Acetonitrile → 845617-09-6

HRID 32775Notes

Reaction equation

HRID 32775 reaction equation
ClN1[N:7]=[C:6]([Cl:8])C=CN1.[CH2:9]([N:11]([CH2:14]C)CC)C.[C:16]([N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1)([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17].C(OCC)(=O)C.C(#[N:37])C>[Cl-].[Na+].O>[C:19]([O:18][C:16]([N:23]1[CH2:24][CH2:25][N:26]([C:9]2[N:7]=[C:6]([Cl:8])[N:37]=[CH:14][N:11]=2)[CH2:27][CH2:28]1)=[O:17])([CH3:22])([CH3:21])[CH3:20]

Participants

7

Reactant 5

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 178478418HCID 178478418, compound

Product 1

HCID 86600711845617-09-6

Reagents, catalysts & solvents 1

HCID 57417360Sodium chloride; waterSolvent

Conditions

Temperature
0 °C

Procedure

A solution of 11 mmol of 2,4-dichlorotriazine (WO 02/083654) in 20 ml of acetonitrile was chilled and treated with 11 mmol of triethylamine and 11 mmol of N-BOC-piperazine. The reaction mixture was stirred for 2 hours at 0° C. then for 2 hours at room temperature. Addition of 100 ml brine and extraction with ethyl acetate yielded the crude product which was purified through trituration in ethyl acetate. MS (m/e): 300.3 (MH+, 100%)

Workup

  1. waitfor 2 hours at room temperature

Sources & evidence

ORD record
ord-fdd7a5d52699420ba2d429cc91c66bbc
Source dataset
uspto-grants-2008_09
Patent number
US07427612B2

Reaction notes

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