Sodium Hydroxide → HCID 13151893, compound

HRID 1075014Notes

Reaction equation

HRID 1075014 reaction equation
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2S[C:12]3[CH:14]=[C:15]([C:18]([OH:20])=[O:19])[CH:16]=[CH:17][C:11]=3[CH2:10][CH2:9][C:8]=2[CH:21]=1)(=[O:3])C.[OH-:22].[Na+].[S:24](S([O-])=O)([O-:27])(=O)=[O:25].[Na+].[Na+]>Cl[O-].[Na+]>[CH:17]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:21]=[C:4]([C:1]([OH:3])=[O:22])[CH:5]=[CH:6][C:7]=3[S:24](=[O:27])(=[O:25])[C:12]=2[CH:14]=[C:15]([C:18]([OH:20])=[O:19])[CH:16]=1

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 656671Sodium PyrosulfiteHCID 13151869HCID 13151869, compound

Product 1

HCID 13151893HCID 13151893, compound

Reagents, catalysts & solvents 1

HCID 23665760Sodium HypochloriteSolvent

Conditions

Temperature
75 °C

Procedure

Add 2 g. of 8-acetyl-10,11-dihydrodibenzo[b,f]thiepin-3-carboxylic acid to a stirred solution of 50% sodium hypochlorite (400 ml.) and 15 ml. of 20% aqueous sodium hydroxide at 60° C. Heat for 48 hours at 75° C. Cool to room temperature and add sodium metabisulfite. Acidify and separate the solids by filtration. Purify by chromotography over silica gel eluting with a mixture of 80 parts toluene, 20 parts dioxane and 4 parts acetic acid. (m.p.~375° C.)

Workup

  1. additionAdd 2 g
  2. customat 60° C
  3. temperatureCool to room temperature
  4. customseparate the solids
  5. filtrationby filtration
  6. customPurify by chromotography over silica gel eluting with a mixture of 80 parts toluene, 20 parts dioxane and 4 parts acetic acid

Sources & evidence

ORD record
ord-cdfe59cc946447279678260d6459d16f
Source dataset
uspto-grants-1983_07
Patent number
US04394515

Reaction notes

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