Sulfuric Acid → HCID 70482362, compound

HRID 464761Notes

Reaction equation

HRID 464761 reaction equation
C(O)(=O)C.[CH3:5][O:6][C:7]1[CH:32]=[CH:31][C:10]([CH2:11][CH2:12][CH:13]2[CH2:17][CH2:16][CH:15]([C:18]3[CH:19]=[CH:20][C:21]4[O:25][C:24]([CH3:27])([CH3:26])[S:23][C:22]=4[CH:28]=3)[N:14]2[CH2:29][OH:30])=[CH:9][CH:8]=1.[S:33](=[O:37])(=[O:36])([OH:35])[OH:34]>C(O)C>[S:33](=[O:35])(=[O:34])([OH:37])[OH:36].[CH3:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:11][CH2:12][CH:13]2[CH2:17][CH2:16][CH:15]([C:18]3[CH:19]=[CH:20][C:21]4[O:25][C:24]([CH3:27])([CH3:26])[S:23][C:22]=4[CH:28]=3)[N:14]2[CH2:29][OH:30])=[CH:31][CH:32]=1

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 20262543HCID 20262543, compound

Product 1

HCID 70482362HCID 70482362, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

2-(p-methoxyphenethyl)-5-(2,2-dimethyl-1,3-benzoxathiol-5-yl)hydroxymethylpyrrolidine acetate prepared according to Example 6.B. (1.0 g) is dissolved in a solution of 1 ml 50% aqueous sulfuric acid in 10 ml ethanol and the resulting precipitate harvested. The product is suspended in ethanol and filtered, air dried, and recrystallized from methanol/acetone to yield 2-(p-methoxyphenethyl)-5-(2,2-dimethyl-1,3-benzoxathiol-5-yl)hydroxymethylpyrrolidine bisulfate.

Workup

  1. filtrationfiltered
  2. customair dried
  3. customrecrystallized from methanol/acetone

Sources & evidence

ORD record
ord-55a355b53b8e48c7b71143269f9abe16
Source dataset
uspto-grants-1985_10
Patent number
US04548951

Reaction notes

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