Sulfuric Acid → HCID 23460472, compound

HRID 2286869Notes

Reaction equation

HRID 2286869 reaction equation
[Cl:1][C:2]([Cl:15])([Cl:14])[CH:3]1[NH:8][C:7](=O)[C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1.[Cl-].[Na+].[S:18](=O)(=[O:21])([OH:20])[OH:19]>>[Cl:1][C:2]([Cl:15])([Cl:14])[CH:3]1[NH:8][CH2:7][C:6]2[CH:10]=[C:11]([S:18]([OH:21])(=[O:20])=[O:19])[CH:12]=[CH:13][C:5]=2[O:4]1

Participants

4

Reactant 3

HCID 1118Sulfuric AcidHCID 5234Sodium ChlorideHCID 590558HCID 590558, compound

Product 1

HCID 23460472HCID 23460472, compound

Procedure

A mixture of 3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazin-4-one (10 g.--obtained as described in Example 3) and concentrated sulphuric acid (100 ml.) was heated on a steam bath for 18 hours, and drowned into ice (400 g.). The resulting solution was saturated with sodium chloride and extracted with ethyl acetae (4×100 ml.) The extracts were combined and dried, the solvent was evaporated, and the residue was crystallised from glacial acetic acid to give 3,4-dihydro-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-sulphonic acid, m.p. > 260° C.

Workup

  1. temperaturewas heated on a steam bath for 18 hours
  2. extractionextracted with ethyl acetae (4×100 ml.) The extracts
  3. customdried
  4. customthe solvent was evaporated
  5. customthe residue was crystallised from glacial acetic acid

Sources & evidence

ORD record
ord-f694c8868056415fb5b5246fc6c0ffa1
Source dataset
uspto-grants-1981_05
Patent number
US04268510

Reaction notes

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