Water → HCID 13017871, compound

HRID 1578042Notes

Reaction equation

HRID 1578042 reaction equation
[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]3([CH2:20][CH2:19][C:18](=O)[CH2:17][CH2:16]3)[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH2:22].O.O.C([O-])(=O)C.[Na+].Cl.[NH2:31]O.O>C(O)C>[N:31](=[C:18]1[CH2:17][CH2:16][C:9]2([C:6]3[C:1](=[CH:2][CH:3]=[CH:4][CH:5]=3)[CH:7]([C:15]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)[O:8]2)[CH2:20][CH2:19]1)[OH:22]

Participants

6

Reactant 4

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 13017870HCID 13017870, compoundHCID 23665404Sodium Acetate Trihydrate

Product 1

HCID 13017871HCID 13017871, compoundYield 92.3%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A warm solution of 8.35 g of 3'-phenylspiro[cyclohexane-1,1'(3'H)-isobenzofuran]-4-one in 300 ml of ethanol is mixed with a solution of 8.16 g of sodium acetate trihydrate, 4.17 g of hydroxylamine hydrochloride, and 60 ml of water. The solution is refluxed for 120 minutes. The solvent is removed in vacuo and the residue stirred with 300 ml of water. The precipitate is suction filtered, washed with water and dried to give 92.3% of product, mp: 172°-175° C.

Workup

  1. temperatureThe solution is refluxed for 120 minutes
  2. customThe solvent is removed in vacuo
  3. filtrationfiltered
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-74eb5d6ae9a942e399222e0e4f8a2388
Source dataset
uspto-grants-1981_09
Patent number
US04290958

Reaction notes

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