Benzyl Alcohol → HCID 13043363, compound

HRID 1633005Notes

Reaction equation

HRID 1633005 reaction equation
[CH2:1]([OH:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Na].[Cl:10][C:11]1[N:12]=[C:13]([N:22]2[CH2:27][CH2:26][S:25](=[O:28])[CH2:24][CH2:23]2)[C:14]2[N:20]=[CH:19][N:18]=[C:17](Cl)[C:15]=2[N:16]=1>C1C=CC=CC=1.O1CCOCC1>[CH2:1]([O:8][C:17]1[C:15]2[N:16]=[C:11]([Cl:10])[N:12]=[C:13]([N:22]3[CH2:23][CH2:24][S:25](=[O:28])[CH2:26][CH2:27]3)[C:14]=2[N:20]=[CH:19][N:18]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

6

Reactant 3

HCID 244Benzyl AlcoholHCID 5360545SodiumHCID 128169922,8-Dichloro-4-(1-oxido-thiomorpholino)-pyrimido[5,4-d]pyrimidine

Product 1

HCID 13043363HCID 13043363, compound

Reagents, catalysts & solvents 2

HCID 241BenzeneSolventHCID 312751,4-DioxaneSolvent

Procedure

An alcoholate solution, prepared from 22 gm (0.2 mol) of benzyl alcohol in 100 ml of absolute benzene with 1.6 gm (0.07 mol) of sodium, was added to a solution of 15.9 gm (0.05 mol) of 2,8-dichloro-4-(1-oxido-thiomorpholino)pyrimido[5,4-d]-pyrimidine in 400 ml of dioxane at about 30° C., and the mixture thus obtained was stirred at room temperature for about two hours. The reaction mixture was then evaporated in vacuo, and the residue was admixed with about 500 ml of water. The precipitate which solidified after standing for a short time, was filtered off, washed with water and dried at about 70° C.

Workup

  1. customthe mixture thus obtained
  2. customThe reaction mixture was then evaporated in vacuo
  3. filtrationwas filtered off
  4. washwashed with water
  5. customdried at about 70° C.

Sources & evidence

ORD record
ord-e5255767a5e341cc84a7e1a84c2f5b94
Source dataset
uspto-grants-1984_10
Patent number
US04478833

Reaction notes

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