Water → HCID 19068971, compound

HRID 1957212Notes

Reaction equation

HRID 1957212 reaction equation
[Al+3].[Cl-].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[CH3:9][N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]2[CH:19]=[C:20]([C:22]([O:24][CH3:25])=[O:23])[S:21][C:11]1=2.O>ClCCCl>[C:5]([C:15]1[CH:14]=[C:13]2[C:18](=[CH:17][CH:16]=1)[N:10]([CH3:9])[C:11]1[S:21][C:20]([C:22]([O:24][CH3:25])=[O:23])=[CH:19][C:12]2=1)(=[O:7])[CH3:6]

Participants

6

Reactant 4

HCID 962WaterHCID 6367Acetyl chloride2×HCID 1474903HCID 1474903, compoundHCID 6451240Aluminum(III) Chloride2×

Product 1

HCID 19068971HCID 19068971, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Procedure

To a slurry of 870 mg AlCl3 in 50 ml dry 1,2-dichloroethane was added 465 μl acetyl chloride. The mixture was stirred for 30 min. at room temperature. 800 mg of (6) was added, and stirring continued overnight. Another 870 mg AlCl3 and 465 μl acetyl chloride was added, and stirring continued overnight. Water was added, and the organic phase dried and evaporated to dryness giving a brown powder, which was crystallized from acetic acid and petrol ether giving (64). Yield 210 mg. M. p. 196°-8° C.

Workup

  1. stirringstirring continued overnight
  2. stirringstirring continued overnight
  3. customthe organic phase dried
  4. customevaporated to dryness
  5. customgiving a brown powder, which
  6. customwas crystallized from acetic acid and petrol ether giving (64)

Sources & evidence

ORD record
ord-d477789eaa3e4591bd9fbc95f46780f5
Source dataset
uspto-grants-1998_07
Patent number
US05783575

Reaction notes

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