Sodium Sulfite → HCID 15723443, compound

HRID 625708Notes

Reaction equation

HRID 625708 reaction equation
C1(S[C:8]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:9]=2[CH2:10][CH2:11][C:12]3=[O:17])C=CC=CC=1.Cl[C:19]1[CH:20]=[C:21]([CH:26]=[CH:27][CH:28]=1)C(OO)=O.[S:29]([O-:32])([O-])=[O:30].[Na+].[Na+]>ClCCl>[C:19]1([S:29]([C:8]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:9]=2[CH2:10][CH2:11][C:12]3=[O:17])(=[O:32])=[O:30])[CH:20]=[CH:21][CH:26]=[CH:27][CH:28]=1

Participants

5

Procedure

The material from Step 1 (0.34 g) is allowed to react with 3-chloroperoxybenzoic acid (0.73 g) in dichloromethane (5 mL) with stirring for 1 hour. The mixture is diluted with dichloromethane, 5% aqueous sodium sulfite solution is added and stirred vigorously for 10 minutes. The phases are separated, the organic phase washed with NaOH solution (0.2 M), dried and the solvent removed to give the desired material (0.39 g). LC (METHOD 5): tR=0.98 min; Mass spectrum: m/z=290 [M+NH4]+.

Workup

  1. additionis added
  2. stirringstirred vigorously for 10 minutes
  3. customThe phases are separated
  4. washthe organic phase washed with NaOH solution (0.2 M)
  5. customdried
  6. customthe solvent removed

Sources & evidence

ORD record
ord-03aae4d0b9b944809019f92fbc06f99c
Source dataset
uspto-grants-2016_04
Patent number
US09308194B2

Reaction notes

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