Potassium Acetate → 7-Methoxy-3-{1-[5-(4-methyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-6-oxo-5.6-dihydro-pyridazin-3-yl]-piperidin-4-yl}-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

HRID 469395Notes

Reaction equation

HRID 469395 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:44]=[C:43]([CH3:45])[C:38]2[NH:39][C:40](=[O:42])[O:41][C:37]=2[CH:36]=1)=[O:34]>C(O)(=O)C>[CH3:31][O:30][C:27]1[CH:28]=[CH:29][C:22]2[NH:21][C:20](=[O:32])[N:19]([CH:16]3[CH2:15][CH2:14][N:13]([C:10]4[N:11]=[N:12][C:7](=[O:3])[CH:8]([C:33]([C:35]5[CH:44]=[C:43]([CH3:45])[C:38]6[NH:39][C:40](=[O:42])[O:41][C:37]=6[CH:36]=5)=[O:34])[CH:9]=4)[CH2:18][CH2:17]3)[CH2:25][CH2:24][C:23]=2[CH:26]=1

Participants

4

Reactant 2

HCID 517044Potassium AcetateHCID 252694613-{1-[6-Chloro-5-(4-methyl-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 252698057-Methoxy-3-{1-[5-(4-methyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-6-oxo-5.6-dihydro-pyridazin-3-yl]-piperidin-4-yl}-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

0.10 g (1.0 mmol) potassium acetate were added to 0.13 g (0.20 mmol) 3-{1-[6-chloro-5-(4-methyl-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 3 mL acetic acid and the mixture was boiled under a nitrogen atmosphere for 7 h. Then the reaction mixture was evaporated down and the residue was triturated with water, suction filtered and dried. The residue was purified by preparative HPLC-MS. The fractions containing the product were combined and freeze-dried.

Workup

  1. customThen the reaction mixture was evaporated down
  2. customthe residue was triturated with water, suction
  3. filtrationfiltered
  4. customdried
  5. customThe residue was purified by preparative HPLC-MS
  6. additionThe fractions containing the product
  7. customfreeze-dried

Sources & evidence

ORD record
ord-d044d02f032e4ffa85345db1e3b7ebf4
Source dataset
uspto-grants-2014_01
Patent number
US08629137B2

Reaction notes

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