Acetic Anhydride → HCID 86743121, compound

HRID 1607656Notes

Reaction equation

HRID 1607656 reaction equation
[N+:1]([C:4]1[CH:5]=[C:6]([CH:20]=[CH:21][C:22]=1[Cl:23])[C:7]([CH:9]1[CH2:14][C:13]([CH3:16])([CH3:15])[N:12](N)[C:11]([CH3:19])([CH3:18])[CH2:10]1)=[O:8])([O-:3])=[O:2].[C:24]([O:27]C(=O)C)(=O)[CH3:25].C([N:33](CC)CC)C>>[N+:1]([C:4]1[CH:5]=[C:6]([CH:20]=[CH:21][C:22]=1[Cl:23])[C:7]([CH:9]1[CH2:14][C:13]([CH3:16])([CH3:15])[N:12]([C:24](=[O:27])[CH3:25])[C:11]([CH3:19])([CH3:18])[CH:10]1[NH2:33])=[O:8])([O-:3])=[O:2]

Participants

4

Reactant 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 86743122HCID 86743122, compound

Product 1

HCID 86743121HCID 86743121, compound

Procedure

68 Parts of 4-(3'-nitro-4'-chlorobenzoyl)-amino-2,2,6,6-tetramethylpiperidine are added to 250 parts of acetic anhydride. After the addition of 21 parts of triethylamine, the suspension is stirred for 16 hours at toom temperature and then for 3 hours at 100°-110°. In order to complete precipitation of the acetyl derivative, 1500 parts by volume of cold water are added and stirred at room temperature until all the excess acetic anhydride is destroyed. The precipitate is then filtered, washed neutral with water and dried. 72 parts of 4-(3'-nitro-4'-chlorobenzoyl)-amino-1-acetyl-2,2,6,6-tetramethyl-piperidine having a melting point of 198°-200° results.

Workup

  1. waitfor 3 hours at 100°-110°
  2. customprecipitation of the acetyl derivative, 1500 parts by volume of cold water
  3. additionare added
  4. stirringstirred at room temperature until all the excess acetic anhydride
  5. customis destroyed
  6. filtrationThe precipitate is then filtered
  7. washwashed neutral with water
  8. customdried

Sources & evidence

ORD record
ord-cae37c96478742fba79b28cd55e12e04
Source dataset
uspto-grants-1989_09
Patent number
US04866113

Reaction notes

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