Acetyl chloride → HCID 23332945, compound

HRID 224397Notes

Reaction equation

HRID 224397 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]([NH2:20])[C:5]2[O:10][CH:9]([C:11]([Cl:14])([Cl:13])[Cl:12])[O:8][CH:7]([C:15]([Cl:18])([Cl:17])[Cl:16])[C:6]=2[CH:19]=1.C(O[C:25](=[O:27])[CH3:26])(=O)C.[C:28](Cl)(=[O:30])[CH3:29]>>[C:28]([N:1]([C:25](=[O:27])[CH3:26])[C:2]1[CH:3]=[C:4]([N:20]([C:9](=[O:10])[CH3:11])[C:7](=[O:8])[CH3:6])[C:5]2[O:10][CH:9]([C:11]([Cl:12])([Cl:13])[Cl:14])[O:8][CH:7]([C:15]([Cl:18])([Cl:17])[Cl:16])[C:6]=2[CH:19]=1)(=[O:30])[CH3:29]

Participants

4

Procedure

A mixture of 6,8-diamino-2,4-bis(trichloromethyl)benzo[1,3]dioxin (1 g.), acetic anhydride (25 ml.) and acetyl chloride (2 ml.) was heated on the steam bath for 10 hours. After cooling, the reaction mixture was evaporated to dryness under reduced pressure, and the residue was triturated with aqueous ethanol. The solid product thus obtained was crystallised from ethanol to give 6,8-bis(diacetylamino)-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 182°-183° C.

Workup

  1. temperaturewas heated on the steam bath for 10 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated to dryness under reduced pressure
  4. customthe residue was triturated with aqueous ethanol
  5. customThe solid product thus obtained
  6. customwas crystallised from ethanol

Sources & evidence

ORD record
ord-b0f3511aaaef4f9ca20e9f197493c9e0
Source dataset
uspto-grants-1980_11
Patent number
US04232032

Reaction notes

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