Water → HCID 13017871, compound

HRID 1577675Notes

Reaction equation

HRID 1577675 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-7622915f43f94d589095dad8b3560863
Source dataset
uspto-grants-1981_09
Patent number
US04288623

Reaction notes

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