Iodoethanol → HCID 19047275, compound

HRID 1780658Notes

Reaction equation

HRID 1780658 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)[CH2:4][CH2:3]1.[I:17][CH2:18][CH2:19][OH:20]>CN(C=O)C>[I-:17].[OH:20][CH2:19][CH2:18][N+:2]1([CH3:1])[CH2:3][CH2:4][N:5]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)[CH2:6][CH2:7]1

Participants

4

Reactant 2

HCID 12225Iodoethanol2×HCID 37945392-(4-methylpiperazino)-1,3-benzoxazole

Product 1

HCID 19047275HCID 19047275, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A 435 mg portion of 2-(4-methyl-1-piperazinyl)-benzoxazole was dissolved in 3 ml of DMF. Under cooling with ice, 0.24 ml of 2-iodoethyl alcohol was added to the thus prepared solution, and the reaction was carried out for 1 hour at the same temperature and then for 17 hours at room temperature, followed by further addition of 0.48 ml 2 -iodoethyl alcohol and subsequent 21 hours of reaction at 50° C. The reaction mixture was concentrated under a reduced pressure, and 5 ml of acetone was added to the resulting residue. The precipitate thus formed was collected by filtration, washed with acetone and then dried to obtain 583 mg of the title compound.

Workup

  1. additionwas added to the thus prepared solution
  2. waitfor 17 hours at room temperature
  3. concentrationThe reaction mixture was concentrated under a reduced pressure, and 5 ml of acetone
  4. additionwas added to the resulting residue
  5. customThe precipitate thus formed
  6. filtrationwas collected by filtration
  7. washwashed with acetone
  8. customdried

Sources & evidence

ORD record
ord-96c597d43d66453d917d5acd2c43336c
Source dataset
uspto-grants-1997_05
Patent number
US05631257

Reaction notes

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