Sulfuric Acid → HCID 23690675, compound

HRID 1982174Notes

Reaction equation

HRID 1982174 reaction equation
C(OC(=O)C)(=O)C.[CH3:8][C:9]1[C:18]2[C:12]([CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[CH:11][CH:10]=1.[S:19](=O)(=[O:22])([OH:21])[OH:20].[OH-].[Na+:25]>>[CH3:8][C:9]1[CH:10]=[C:11]([S:19]([O-:22])(=[O:21])=[O:20])[C:12]2[C:18]=1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2.[Na+:25]

Participants

5

Reactant 4

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 1366111-Methylazulene

Product 1

HCID 23690675HCID 23690675, compound

Conditions

Temperature
0 °C

Procedure

Acetic anhydride in an amount of 10 ml is added to 1.0 g. of 1-methylazulene under cooling with ice-water, sulfuric acid in an amount of 3.4 g. is added dropwise and the reaction mixture is stirred for 4 hours at 0° C. Then, the reaction mixture is alkalized to pH8-9 by adding 40% of sodium hydroxide solution and the generated solid is collected and dried. The product is recrystalized from 95% ethanol to give 1.1 g. of the objective compound.

Workup

  1. additionis added dropwise
  2. customthe generated solid is collected
  3. customdried
  4. customThe product is recrystalized from 95% ethanol
  5. customto give 1.1 g

Sources & evidence

ORD record
ord-1d1769a5861f45b4ac2a6aa93ad0e752
Source dataset
uspto-grants-1986_06
Patent number
US04595694

Reaction notes

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