Acetic Anhydride → HCID 23471620, compound

HRID 128013Notes

Reaction equation

HRID 128013 reaction equation
[CH3:1][CH:2]1[C:7]([C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[NH:13][CH2:12][CH2:11]3)=[N:6][NH:5][C:4](=[O:17])[CH2:3]1.C(N(CC)CC)C.[C:25](OC(=O)C)(=[O:27])[CH3:26]>C(Cl)(Cl)Cl>[CH3:1][CH:2]1[C:7]([C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[N:13]([C:25](=[O:27])[CH3:26])[CH2:12][CH2:11]3)=[N:6][NH:5][C:4](=[O:17])[CH2:3]1

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 23471618HCID 23471618, compound

Product 1

HCID 23471620HCID 23471620, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

To a solution of 5-(5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)indoline in 100 ml of chloroform was added 5 ml of triethylamine with stirring. To the mixture was added dropwise 3 ml of acetic anhydride. After maintaining at room temperature for one hour, the reaction mixture was concentrated under reduced pressure. The residual crystals were filtered off, washed with water and recrystallized from ethanol to give 4.3 g of 5-(5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)-1-acetylindoline as white crystals, melting at 258°-261° C.

Workup

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. filtrationThe residual crystals were filtered off
  3. washwashed with water
  4. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-244f7a2d20454e34933c5944740d6b15
Source dataset
uspto-grants-1981_03
Patent number
US04258185

Reaction notes

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