Potassium Acetate → 3-{1-[5-(3,4-Dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-6-oxo-1,6-dihydro-pyridazin-3-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

HRID 469396Notes

Reaction equation

HRID 469396 reaction equation
C([O-])(=[O:3])C.[K+].Cl[C:7]1[N:12]=[N:11][C:10]([N:13]2[CH2:18][CH2:17][CH:16]([N:19]3[CH2:25][CH2:24][C:23]4[CH:26]=[C:27]([O:30][CH3:31])[CH:28]=[CH:29][C:22]=4[NH:21][C:20]3=[O:32])[CH2:15][CH2:14]2)=[CH:9][C:8]=1[C:33]([C:35]1[CH:45]=[C:44]([CH3:46])[C:38]2[N:39]([CH3:43])[C:40](=[O:42])[O:41][C:37]=2[CH:36]=1)=[O:34]>C(O)(=O)C>[CH3:43][N:39]1[C:38]2[C:44]([CH3:46])=[CH:45][C:35]([C:33]([C:8]3[C:7](=[O:3])[NH:12][N:11]=[C:10]([N:13]4[CH2:14][CH2:15][CH:16]([N:19]5[CH2:25][CH2:24][C:23]6[CH:26]=[C:27]([O:30][CH3:31])[CH:28]=[CH:29][C:22]=6[NH:21][C:20]5=[O:32])[CH2:17][CH2:18]4)[CH:9]=3)=[O:34])=[CH:36][C:37]=2[O:41][C:40]1=[O:42]

Participants

4

Reactant 2

HCID 517044Potassium AcetateHCID 252708103-{1-[6-Chloro-5-(3,4-dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-pyridazin-3-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

Product 1

HCID 698126363-{1-[5-(3,4-Dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-6-oxo-1,6-dihydro-pyridazin-3-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

0.10 g (1.02 mmol) potassium acetate were added to 0.13 g (0.20 mmol) 3-{1-[6-chloro-5-(3,4-dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-pyridazin-3-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one (mixture) in 2 mL acetic acid and the mixture was boiled for 16 h under a nitrogen atmosphere. Then the reaction mixture was purified by preparative HPLC-MS. The fractions containing the product were combined and freeze-dried.

Workup

  1. customThen the reaction mixture was purified by preparative HPLC-MS
  2. additionThe fractions containing the product
  3. customfreeze-dried

Sources & evidence

ORD record
ord-fc68219d711746cabead25bac6d7eb59
Source dataset
uspto-grants-2014_01
Patent number
US08629137B2

Reaction notes

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