Acetonitrile → 845617-09-6

HRID 1820754Notes

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

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

waitfor 2 hours at room temperature

Sources & evidence

ORD record: ord-92db4547c0e34f6eb7e131b24cc3ed08
Source dataset: uspto-grants-2009_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07605163B2

Reaction notes

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